反应详情

1.1 g of triethyl amine was added to a suspension of 1.0 g of 1-oxo-1,2,3,4-tetrahydro-3-isoquinoline carboxylic acid in 10 ml of acetonitrile. A solution of 3-acetylthiopropionyl chloride (3-acethylthiopropionyl chloride was prepared by adding 1.0 g of thionyl chloride to a solution of 0.8 g of 3-acetylthiopropionic acid in 5 ml of benzene, stirring the solution overnight at room temperature and distilling off the solvent and excess thionyl chloride) in 5 ml of acetonitrile was added drop by drop to the suspension which was ice-cooled. After stirring the mixture for 2 hours at room temperature, the solvent was distilled off, 20 ml of ethylacetate and 10 ml of water were added to the residue and the solution was shaken and the organic phase separated and washed. The organic phase was dried over anhydrous Glauber's salt, the solvent was distilled off and then the residue was recrystalized from benzene to obtain 0.9 g of 2-(3-acetylthiopropionyl)-1-oxo-1,2,3,4-tetrahydro- 3-isoquinoline carboxylic acid as a colorless microcrystalline material.

1. distillationdistilling off the solvent and excess thionyl chloride) in 5 ml of acetonitrile
2. additionwas added drop by drop to the suspension which
3. temperaturecooled
4. stirringAfter stirring the mixture for 2 hours at room temperature
5. distillationthe solvent was distilled off
6. addition20 ml of ethylacetate and 10 ml of water were added to the residue
7. stirringthe solution was shaken
8. customthe organic phase separated
9. washwashed
10. dry with materialThe organic phase was dried over anhydrous Glauber's salt
11. distillationthe solvent was distilled off
12. customthe residue was recrystalized from benzene