반응 #2383770

반응 방정식

water

lithium aluminum hydride

S-methyl-thioglycolic acid-N-(2-methylthioethyl)-amide

S-methyl-thioglycolic Acid-N-(2-methylthioethyl)-amide

water

lithium aluminum hydride

→

bis-(2-methylthioethyl)-amine

용매

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   온도Then, it is refluxed for 18 hours
2. 2
   온도While being cooled in an ice bath
3. 3
   추출The solution is extracted three times with methylene chloride/methanol 10/1
4. 4
   세척the combined organic phases are washed with water one time
5. 5
   농축After concentration
6. 6
   기타by evaporation
7. 7
   기타the residue is purified by chromatography with the mobile solvent system of methylene chloride/methanol

실험 절차

5.18 g of S-methyl-thioglycolic acid-N-(2-methylthioethyl)-amide (Example 8a) is dissolved in 350 ml of tetrahydrofuran and added in drops to a suspension of 5.48 g of lithium aluminum hydride in 350 ml of tetrahydrofuran under a cover-gas atmosphere. Then, it is refluxed for 18 hours. While being cooled in an ice bath, the excess lithium aluminum hydride is carefully hydrolyzed by adding 100 ml of water in drops, it is stirred for 1 more hour, and then another 700 ml of water is added. The solution is extracted three times with methylene chloride/methanol 10/1, and the combined organic phases are washed with water one time. After concentration by evaporation, the residue is purified by chromatography with the mobile solvent system of methylene chloride/methanol: yield 1.5 g=32% of theory.

출처