HRID15362

反应详情

EQUATION

反应方程式

HRID 15362 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 7-bromo-2,3-dihydro-1-benzofuran-5-carbaldehyde (1.3 g, 4.7 mmol) in dimethylacetamide (2 mL) was added copper(I) cyanide (0.41 g g, 4.7 mmol). The reaction was refluxed for 18 hours, and then concentrated under reduced pressure. The residue was washed well with warm ethyl acetate. The combined ethyl acetate layer were concentrated and dried. The crude product was purified by flash column chromatography (silica gel, 4:1 and 2:1 hexane:ethyl acetate gradient) to afford the desired product (0.5 g, 50%).

WORKUP

后处理

  1. temperatureThe reaction was refluxed for 18 hours
  2. concentrationconcentrated under reduced pressure
  3. washThe residue was washed well with warm ethyl acetate
  4. concentrationThe combined ethyl acetate layer were concentrated
  5. customdried
  6. customThe crude product was purified by flash column chromatography (silica gel, 4:1 and 2:1 hexane:ethyl acetate gradient)