HRID40101
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- -78 °C
PROCEDURE
实验过程
General Procedure O. To a solution of methyl3-(3,4-difluorobenzylcarbamoyl)-6-methoxy-1-(pyridin-2-ylmethyl)-1H-indole-2-carboxylate (Compound 93, 515 mg, 1.11 mmol) in CH2Cl2 (20 ml) at −78° C. was added DIBAL (1 M in CH2Cl2, 4.4 ml, 4.44 mmol) slowly. The reaction was stirred at −78° C. for 2 h, quenched with H2O, diluted with EtOAc, washed with NaOH and brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by chromatography on silica gel (0→100% EtOAc-hexanes) to yield the title compound as a beige solid.
WORKUP
后处理
- customquenched with H2O
- additiondiluted with EtOAc
- washwashed with NaOH and brine
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo
- customThe residue was purified by chromatography on silica gel (0→100% EtOAc-hexanes)