胆甾-3β,5α,6β-三醇衍生物的合成

Synthesis of Cholesta-3β,5α,6β-triol-3,6-dimonooxalate

研究了胆甾-3β,5α,6β-三醇的水溶性衍生物的合成.以胆固醇为原料在质量分数为88%的甲酸中以质量分数为30%的过氧化氢（H2O2）溶液氧化、甲醇中碱水解得胆甾-3β,5α,6β-三醇,收率83.5%,m.p.228-230℃,再以胆甾-3β,5α,6β-三醇与草酰氯于丙酮中0℃反应15min,吡啶为催化剂,然后加入少量水继续反应约30 min,得胆甾-3β,5α,6β-三醇-3,6-二草酸单酯,收率61.5%,m.p.207-209℃.经IR和1H-NMR确证结构正确。

To produce a derivative of Cholesta-3β,5α,6β-triol Cholesta-3β,5α,6β-triol was synthesized from Cholesterol as rawmaterials through 30 % H2O2 oxidation in 88 % formic acid,and the yield was found to be 83. 5 %,m. p. 228 - 230 ℃. Cholesta-3β,5α,6β-triol-3,6-dimonooxalate was synthesized from Cholestan-3β,5α,6β-triol and oxalyl chloride as rawmaterials esterificating at 0 ℃ in the acetone with pyridine as a catalyst in 15 min and then hydrolysing at 0 ℃ in 30 min by addition of a little water.The yield was found to be 61. 5 %,m. p. 207 - 209 ℃. The two compounds were corroborated structurally by IR and1H-NMR.