反应详情

温度

-7 °C

To a solution of 100 mg 1-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-2-(1-isopropyl-piperidin-4-ylcarbamoyl)-1H-indole-5-carboxylic acid and 50 μl NEt3 in 4 ml THF, 17 μl ethyl chloroformate were added at −7° C. After stirring for 2 h at −7° C. the reaction mixture was filtered, the filtrate was treated with 24 mg NaBH4 and warmed to room temperature. After 2 h additional 24 mg NaBH4 were added and the reaction mixture stirred for 16 h. Then, 110 μl MeOH in 4 ml THF were added within 2 h and the reaction mixture was stirred for additional 4 h at room temperature. After removal of the solvents under reduced pressure the residue was purified by chromatography on silica gel eluting with DCM/MeOH 8:2. The fractions containing the product were collected and evaporated under reduced pressure.

1. filtrationwas filtered
2. additionthe filtrate was treated with 24 mg NaBH4
3. temperaturewarmed to room temperature
4. additionAfter 2 h additional 24 mg NaBH4 were added
5. stirringthe reaction mixture stirred for 16 h
6. additionThen, 110 μl MeOH in 4 ml THF were added within 2 h
7. stirringthe reaction mixture was stirred for additional 4 h at room temperature
8. customAfter removal of the solvents under reduced pressure the residue
9. customwas purified by chromatography on silica gel eluting with DCM/MeOH 8:2
10. additionThe fractions containing the product
11. customwere collected
12. customevaporated under reduced pressure