反応 #75217

反応方程式

hydrogen

7-thia-13-prostynoic acid

→

semisolid

収率 85.6%

7-Thiaprostanoic Acid

収率 85.6%

溶媒

ethyl acetate

ethyl acetate

反応条件

後処理

1. 1
   その他After 5 hrs the catalyst was removed by filtration
2. 2
   洗浄washed with ethyl acetate
3. 3
   その他the combined filtrates evaporated

実験手順

To a suspension of 50 mg of 10% palladium on charcoal in 1 ml of ethyl acetate, which had been pre-reduced with hydrogen gas was added 7-thia-13-prostynoic acid (15 mg) in 1.5 ml of ethyl acetate. After 5 hrs the catalyst was removed by filtration washed with ethyl acetate and the combined filtrates evaporated to yield 13 mg of a semisolid. Analysis by nmr indicated that there still remained starting material plus some 7-thia-13-cis-prostenoic acid. The material was therefore reduced again with 50 mg of fresh palladium catalyst for 1/2 hour and the reduced material isolated by filtration and removal of the solvent. 8 Milligrams of the saturated acid was obtained, which after recrystallization from hexane melted at 40°-41°.

出典