反应详情

Morpholine (0.107 ml, 1.23 mmol) and the intermediate I2 (239 mg, 1.12 mmol) were dissolved in 5 ml of DMF and cooled in an ice-bath. HOBT (188 mg, 1.23 mmol), triethylamine (0.309 ml, 2.24 mmol) and EDC (214 mg, 1.12 mmol) were added successively. The ice-bath was removed and stirring continued over night. The mixture was evaporated, redissolved in diethyl ether and extracted with 2N-HCl (twice), 5% sodium bicarbonate and brine. The organic layer was dried over anhydrous sodium sulfate and evaporated to give a pale yellow oil. Yield (crude): 320 mg (93%).

1. temperaturecooled in an ice-bath
2. customThe ice-bath was removed
3. waitcontinued over night
4. customThe mixture was evaporated
5. dissolutionredissolved in diethyl ether
6. extractionextracted with 2N-HCl (twice), 5% sodium bicarbonate and brine
7. dry with materialThe organic layer was dried over anhydrous sodium sulfate
8. customevaporated
9. customto give a pale yellow oil
10. customYield (crude)