HRID2228352

反应详情

EQUATION

反应方程式

HRID 2228352 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The above 6-methoxy-3,3-dimethyl-5-prop-2-ynyloxy-indan-1-one (2.44 g) was treated with 1.13 g of ethyl cyano acetate in the presence of 0.1 equivalents of pyrrolidine and benzoic acid in 20 ml of xylene. The reaction mixture was refluxed for 30 hours with simultaneous separation of water. Then, the cold reaction mixture was washed with water, concentrated and chromatographed in hexane/ethyl acetate through SiO2 to yield 0.7 g of yellow crystals. m.p. 132-136° C. UV 362 nm (ε=23′222), MS: 339(M+), 324, 300 (100%).

WORKUP

后处理

  1. customThen, the cold reaction mixture
  2. washwas washed with water
  3. concentrationconcentrated
  4. customchromatographed in hexane/ethyl acetate through SiO2