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Vajor Lars: our : Loth,nJ was ‘ ~ [I n‘n.‘.‘ ‘,: H ’\ ‘\ n" \v‘pfi A ~ 5‘ 3' cone on an AUTVLrLfin moueL A—‘U-P GL0 CMnr autugru a. 7; “A: “I. f ‘ .1. .- 5,.) _ ~r ,r' -, 1 4. .1... _~ L Lihig ;QLLL3 were caveran u on a noLlur now page A V. m I J- I!“ \r‘ n-J" -- ‘ n II J- ‘ moltiLL gOlno dflydra ‘s and are uncorflecped. ‘7' ya \q A 1;—r~-§ r~.- /‘ 1-] r)“ T -: rvjfl't 7’); A ’I’_~ ‘1 A'leJI can “A.“ \- v.55 a¢od A'AOlC Chfiul. "ICL‘ L (Ab bill arrlil’l(lt iv n8 '8ch : .— fi 1 4-: n 1 ‘ ‘r- LorOLnu JuLCal Laooratory, Ann Arqor, L 4“ .174 C- JCTLOLUCd bx L;ann I/icIIigf \ n. {\J O ‘ n'l'. .0 . '1‘ " 11‘ 1‘ B. Concedsat1on 01 F3? wu ic Acid w1tn Formaloenyqe “0 $ A l. RZG-y’keto_3.‘ nwcv:‘m"““*m"lhoflt8dCGJOlC Lei" 8“ iotenu -—-4n~mww.~_~r~.‘- a“ A— ’ *1" r "t"‘* \ 1 L 1 , x \ .' *1 \\i:_'_ kt: 4.xil—o1/’ H Ll-s. 0L1.) \ 114 (3 ‘L\ 1‘1“. To a cool ed (ice—salt) pasty L"ture of '0.0 3. (0.455 moles) of f1 eshly dist1lled pyruvic acid (b.p.§xmbio) and 20.4 g. (0.680 aoles) of paraformaldehvdfi, 48.02 1 of concen- trated sulfuric acid was adeed dTOpWiSG with stirrin3. The ‘ H A, .2 .: +15 _‘11 1, J. . 1. adoi tion was slow enoa3u (1 hr.) to ma1nta1n cat taup213t1rc '4: . LL 1“L- . _ ya; 11on tie so1ution was “ilctco -J to room temperatu"e, heated on a steam bath for 30 m1n., and allowed to stand at room temper re for b d ys. The daLK brown solution (some crystals were present) was then poured ( P- I) U D. H) O W H O) :S‘ H U) CL 5 3. into Boo ml. of water and allowed to s' which time a tan solid p1ecipitated1The mixture was cooled and filtered yielding about 16 g. of crude pros duct (31:), which upon decolorization (Norit) and crystallization from u fl ~ p ' r w- n/ APO ‘Il water y1e1oed 12 3. (457) 01 y» 1; m.1. 290.2;’ (d) (reporteo ex )1; ’ '“5’ U 9 7 u 77v Cm , m.p. 236-2380 ); V; J EtOX 1 2w 6 :14 20A maxm1 ( ’ U)’ ma y 2.2 Pt1V31tiOn19f 2,o_Diketo-3.)-€1Vr”“ovvwetchhentanedioic ‘ I; ' 35‘ \ fl 1".Clu {11.4. :0 1'1: . 1 u. 1: 1‘ . ‘1-.. - 11 ‘ 1 n 1 .1. "z .‘ L”... Etheral d1a2omcthane has uedcd 51011; b0 a cosine ecucr slurry of 4.0 3. of Kaltwasser's acid (XVL; until the diago— N to q J- ‘ r. .1 ’. r\ n ‘ 1.‘ 4' . a L '1')“ metaanol was aOued to issolve tne CT‘SLC ls and thee etLer and er cess diazom ethane were boiled away. Decolorization and —KEr m'p° 970; d 29 725! 0! 28130! 171309 “133:. crystallit' ation from methanol yielded 2.57 g. (563) of XVIII; 1670, 1360 a 1110 ch*; ‘1;sz 229 mu (6 : 14 ,OC 0), 96085“ 300211 (a - 10, 700); nmr (solvent CD013), sin3lets at 5. 33, 6.00 8: 6 M1727 relative areas 2.0 .2. .: 1.0. igglLICaled. for CllHl206: C, 54.99; H. 5.0M; mole. wt., 240. Found: C, 5M.91; H, b.84; mole. wt., 257 East determination). C. Oxidation ofl {altwass er's Acid with Silver Oxide. l. l-Hydroxymet13l_5_earboxy—3—oxaboic3eloi3 1.8]hex no-2—one ()LI). With stirring 11.4 g. of sodium h3drox'1de in 100 ml. of ater was added to a solution of #5.0 g. of silver nitrate in 250 ml. of water and the resulting brown precipitate (A320) was washed tw ice (av de can tation)v Iith 300 .1. portions of boiling water, and collected by suction filtration. The damp silve r ‘ oxide was then added immediately to a mixture of 6. O .(O. 028 moles) of Ka t.. asser's acid (sVll) and 120 ml. of water in a flask, equip ed with t ue-bore stirrer and reflux condenser. The mixture was re; luxed with stirrin a. ( L; V \ time a silver mirror was forms and carbon ioxide evolved. o. 23 The black insoluble material (Ag & excess A320) was removed by filtration and centrifu gatien, and the resulting clear yellow solution was concentrated by means of a rotoevaporator to a volume of about 50 ml. After addition of 5“ H01 dreprise until it no longer precipitated any silver chloride (if an excess of HCl was added the solution could be cleared again by ad- dition of 10% Na2C03),the silver chloride was removed by k' centrifugation and the resultin3 solution was concentrated on a stezun bath until crystals appeared. The light tan solid (2.0 y.% after decolor i'a tion with? Her tand crystallization from aeetor e,yield cd 1.28 3. of VI (26.0f); m.p. 186—1370; 9::: (Fig. 8) 3L40, 3100, 3000-2600 (b). 1775 a 1725 cal; nmr (solvents D20 and acetone d6)' broad singlet at 3.611’relative area 2.14, closely Spaced doublets at 5.35 (J=Q.SCps), 5.68 (9.5). 5.75 (12.5). 6.32 (12.5). 7.95 (5.5) & 8-53'F(5.5). all with relative areas of 1.0. 2. l—Jy7r0"vr vl 5—earbonethoxy— -oxao1cvclo[5.l Olr exane- 2—one (T Ell; Etheral diazomethane was added to an ether slurry of 89.0 mg. of VII, until the solution remained yellow. After Ht nding (1 hr.) the solution as boiled to reriove e: ccess diazo— methane and concentrated until crystals began to appear. Cooling and collection yielded 80.0 mg. of white crystalline XVIII; m.p. 99-1020; VI;‘ 3500, 3100, 2030, 1770 a 1725 oil; "x (CL 011), J 21+ .\ In ., o ”I .- in} ‘0 '4. .‘I‘ 1‘ .U 13.3.0.3. .Ha. 5:,1J4_ 3 .0..- n1\1 .NJ‘.J an, ‘1 \ Iv.r0» AHHFWVV NrflNO'NlimrowvwvtflpuH "O. r.“ ” OH’LKPIH‘J "PK CKJrO|MIInh~IOQPPHQ0-L-I _P...;.-J.A|T.tp (vi-Kr" 5.5» H gufg H».v?} VHOCIV-U Uatfr'if 4‘ \1 ‘1 lfldfl.(.\J-41|W‘ 0“ 1H .ur'k I). (wrtfrrfrcrkwx»r 00m 000. OON. 003 002 oom— Gown ! \\\\\\ om on IL ., w ow . 9W. w v m , N 8 8 D m .. 8 on 8. 8. 0.0— ON. 0.: 0.0— mZO«U_<< 0d OK 0.0 Cd ooom oonu o.n mzomui o6 Gown I. a V 9. w. m V N 8 n m 8 8. n.« 25 singlets at 6.19 and 7.461?with relative areas of 3.0 : 1.0, doublets at 5.25 ( J = 9.5cps>. 5.68 (12.5). 5.75 (9.5). 6.21 (12.5). 7.94 (5.5).& 8.64T (5.5), with relative areas of 1.2 ° 1.0 : 1.1 : 1.1 : 1.0 : 1.0 rGSpectively. D. Permanganate oxidation of l—hydroxymethyl—S—carboxy-3- oxabicyclo[3.l.0]hexane—2-0ne (VII). A mixture consisting of. 300 mg. of VII dissolved in 8.0 ml. of 5? NaOH, 300 m1. of water, and 736 mg. of potas— sium permanganate was refluxed until the permanganate color disappeared (5 hrs.). The MnOZ was removed by filtration, and the resulting clear solution was concentrated (rotoevap— crater) to a volume of a few milliliters,and acidified with 0.485 N H250“ (24 ml.) to a pH of about 2. The solution was then evaporated to dryness on a rotoevaporator, and the re- sulting solid was treated with an ether solution of diazo- methane until the yellow color persisted. After standing (2 hrs.),the excess diazomethane was removed by boiling and the ether solution was washed with 5% NaHCO3 and saturated NaCl solutions, and dried over MgSOu. The MWSOQ was removed by filtration and the solution concentrated to a volume of a few milliliters.Analysis by vapor phase chromatography on a %" x 5' 20% Silicone SE 20 column at 193° gave two fractions with retention times of 8 and ll min. from ether. 26 1. lLj—Dicarbomethoxy-j—oxabicyclo[3.1.01hexanc_2_one (XXXIII). The 8 min. fraction from the vapor phase chromatography was found to be XXXIII: .Vggiu 3090, 2950, 1790, 1735 & 1460 cml; nmr (0014), singlets at 6.23 and 6.271‘ with a combined relative area of 6.5, and doublets at 5.30 (J 2 9.50ps), 5.8“ (9.5), 7.52 (5.0) & 8.45'7 (5.0) with relative areas of 1.1 : 1.2 : 1.0 : 1.1.re5pective1y. 2. 1,1)2,2—Tetracarbomethoxycyclopropane XXKIV. Comparison of the melting point (690) and infrared Spectrum of the 11 min. fraction from vapor phase chromatography with those of an authentic sample of XXXIV showed them to be identical. E. Synthesis of Authentic 1,1,2,2_Tetracarbomethoxycyclo- propane (XXXIV).19 1. Kethylene-bis-malonic Ester XXXV. Freshly distilled diethylmalonate (64 g.),of boiling point 99° (@ 22 mmz,was added dropwise with stirring to a dry flask containing 9.2 o. of sodium dissolved in 300 m1. of Q absolute ethanol (distilled from Ng)?2 To the resulting clear 27 solution 54.0 g. of methylene iodide (CHZIZ) was added drOpwise and the solution refluxed until no longer basic (2 hrs.). The ethanol was removed by distillation, water was added to dissolve the inorganic salts and the organic layer was taken up in ether. The ether layer was washed with water and 5% NaHSO3 and dried over Nazsou. After removing the ethergthe remaining oil was vacuum distilled at 1.0 mm, and the resulting colorless liquid (XXXV) had the following properties: b'p'l.0mm 1520 (reported19 b 192°); Vmax 2980, 2930, 2900, 1750a 1730 cml; nmr 'p'12mm (CClu), quartet at 5.83’? (J 7.0 ops) with relative area of 4.0, and triplets at 6.57 (7.5), 7.64 (7.5), 8.761T(7.0) with relative areas of 1.0 : 1.0 : 6.0. 2. l,142,2—Tetracarboethoxycyclopropane XXXl . A solution of 11.46 g. of XXXV in 50 ml. of benzene was added to a stirred diSpersion of 3.5 g. of 52.85 sodium hydride on mineral oil, in 250 m1. of benzene (dried over NaH). Bromine was then added to the cooled solution (00) until the bromine brown color persisted (2.1 ml. required), and the solution was refluxed for 4 hrs. After cooling)water was added slowly to destroy the excess Nah and the benzene layer was washed with water and 5% NaHSOB. The liquid remaining upon removal of the benzene was vacuum distilled (b.p.lmnl50—166°) and found by nmr analysis to be a mixture of mono—bromo XXXV and the cyclized product XXXVI. The distillate was then added drOpwise to a stirred diSpcrsion of 1.2 g. of 52.87 fish on 28 mineral oil, in 350 m1. of benzene, and refluxed for three days. After refluxing,the material was worked up as before and distil— led. The 135 to 1500 ( @ 1.0mm) fraction was crystallized from a pentane-ether mixture and yielded 3.9 g. of XXXVI (35$). 1 O *5 3100. max Physical prOpcrties: m.p. 43° (reported19 430); 'V 2980, 1740 & 1250 cml; nmr (0014), a quartet at 5.957’(J 7.00p8). a singlet at 8.0817, and a triplet at 8.85’T(J 7.OCps), with relative areas of 4.0 : 1.0 : 6.0. 3. 1,1,2,2-CyclOprOpanetetracarboxylic acid XII. A solution of 2.0 g. of XXXVI in 10 ml. of glyme and 2.29 g. of barium hydroxide in 280 m1. of water were mixed and refluxed until the mixture was no longer basic (2 hrs.). During this time the insoluble barium salt XXXVII precipitated. The solution was acidified with 0.485 N H250“ to a pH of about 2 and allowed to equilibrate, The barium sulfate was removed by filtration, the filtrate was evaporated to dryness (rotoevaporator), and the resulting white solid was taken up in hot methyl ethyl ketone. Concentration, cooling and precipitation by addition of n—hexane yielded 0.66 g. of XII (50%). Physical properties: m.p. 190—2000 with decomposition and C02evolution,(reported20 ~KBr vmax 3300—2500 (b), 1725, 1420, m.p.. 200, 208, 21a, 210-212°); & 1275 cml; nmr (acetone d6)' singlets at -O.9lfand 7.87T’. Thin layer chromatography;using Silica Gel G with ethanol as the eluent, and visualizing by Spraying with a saturated methanolic 29 solution of " Kallinkrodt IndicatAR pH 3-4 ", showed only one acid Spot. 4. 1,1,2l2-Tetracarbomethoxycyclonropane XXXIV. When 100 mg. of XII was treated with excess diazomethane, according to the procedure described previously,and crystallized from ether,30 mg. of XXXIV (20%) was obtained. Physical prOper- ties: m.p. very sharp 69° (reportedzo 71°); 952;“ 3100, 2950, 17u0, 1435, 1370, 1200 a 1110 cal; nmr (0014), two singlets at 6.23 and 7.821'with relative areas of 6.1 : 1.0. vapor phase chromatography of XXXIV in an ether solution,using a 20% Silicone SE 20 column at 193°, showed only one peak (retention time 11 min. from ether). Comparison ( infrared and m.p.) of the injected and collected material showed them to be identical. 9. 10. 11. 12. l3. 14. 15. l6. 17. 18. 19. 30 LITERATURE CITED 0. Kaltwasser, Ber., 22, 2273 (1896). E. Asahina & S.Terada. J. Pharm. Soc. (Japan), No. 502, 855 (1923)- E. Erlenmeyer, Ber., 32, 1450 (1899). V. Feofilaktov, J. Russ. Phys. Chem. Soc., 61, 1145 (1929). A. I. Scott, Quart. Revs., 12, 1 (1965). P. Bladon, et. al., J. Chem. Soc., 5727 (1963). L. wolrf, Ann., 315, 145 (1901). A. 1. Scott, "Interpretation of the Ultraviolet Spectra of Natural Products", Macmillan, New York, 1964, pp. 58, 79, 238, 241. L. Haynes & J. Plimmer, Quart. Revs., 14, 292 (1960). R. Herbert & E. Hirst, Biochem. J., 22, 1881 (1935). E. R. Jones a M. C. Whiting, J. Chem. Soc., 1419 (1949); 1207 (1953). H. Hift & H. Mahler, J. B101. Chem., 12g, 901 (1952). H. Schinz & M. Hinder, Helv. Chim. Acta., 39, 1349 (1947). C. Djerassi & W. Rittel, J. Amer. Chem. Soc., Z2, 3528 (1957). 0. Brooks & G. Eglinton, et. al., J. Chem. Soc., 308 (1961). T. A. Geissman, J. Amer. Chem. Soc., 25, 4008 (1953). A. w. deJong, Rec. Trav. Chim. Pay-Bas.. 21, 191 (1902). N. Bhacca & D. Williams, "Applications of NNR SpectrOSCOpy in Organic Chemistry", Holden Day, San Francisco, 1964. 0. Dressel, Ann., 256, 174 (1890). 31 20. F. Beilstein, "Handbuch Der Organischen Chemiev Springer- Verlag, Berlin, System No. 1021 (H 990). 21. F. Arndt, Org. Syn., Coll. Vol. II, p. 165. 22. A. ngel, "A Textbook of Practical Organic Chemistry", Longmans, London, 1957. p.167. ”711171111111 19111 l1 1111117 11111111 I!“