反应详情

温度

35 °C

A mixture of 1-benzyl-1,2,3,4-tetrahydroquinolin-7-ol (800 mg, 3.34 mM) and triethylamine (0.5 mL) in dry tetrahydrofuran (THF, 5 ml) was stirred for half an hour under nitrogen atmosphere at room temperature (35° C.). To the stirred reaction mixture, 4-fluorophenyl isocyanate (570 mg/ml, 5.01 mM) was added at once and then the reaction mixture was further stirred for 72 hours under N2 atmosphere at RT. The reaction mixture was concentrated under vacuum and then was quenched with distilled water (1 mL) followed by the extraction with chloroform (3×15 mL). The combined fractions of chloroform was again washed with water and dried over sodium sulphate. Further concentration of chloroform fraction under vacuum afforded the crude product, which was cystallize with methanol-ether (1:5) to yield 8d as solid. Yield: 1.06 g, 84.23%.

1. additionwas added at once and then the reaction mixture
2. stirringwas further stirred for 72 hours under N2 atmosphere at RT
3. concentrationThe reaction mixture was concentrated under vacuum
4. customwas quenched with distilled water (1 mL)
5. extractionfollowed by the extraction with chloroform (3×15 mL)
6. washThe combined fractions of chloroform was again washed with water
7. dry with materialdried over sodium sulphate
8. customFurther concentration of chloroform fraction under vacuum afforded the crude product, which