HRID1506013

反应详情

EQUATION

反应方程式

HRID 1506013 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Lithium aluminium hydride (1M solution in THF, 16.3 mL, 16.3 mmol) was added dropwise to a suspension of 3-bromo-9H-dipyrido[2,3-b;4′,3′-d]pyrrole-6-carboxylic acid methyl ester (500 mg, 1.63 mmol) in THF (10 mL). After 10 minutes the reaction mixture was quenched with a solution of saturated ammonium chloride, diluted with DCM and water and the solid removed by filtration. The layers of the resultant filtrate were separated and the aqueous phase was further extracted with DCM. The combined organic layer was concentrated in vacuo and purified by flash chromatography (silica, 1-15% methanol in DCM).

WORKUP

后处理

  1. customAfter 10 minutes the reaction mixture was quenched with a solution of saturated ammonium chloride
  2. additiondiluted with DCM and water
  3. customthe solid removed by filtration
  4. customThe layers of the resultant filtrate were separated
  5. extractionthe aqueous phase was further extracted with DCM
  6. concentrationThe combined organic layer was concentrated in vacuo
  7. custompurified by flash chromatography (silica, 1-15% methanol in DCM)