HRID1417103

反应详情

EQUATION

反应方程式

HRID 1417103 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A slurry of 2-[4-(2-carboxy-2-methylpropyl)phenoxymethyl]benzoic acid (15.9 g) in 200 ml dry dichloromethane was treated dropwise with 12.5 ml trifluoroacetic anhydride then heated to reflux for 5 hours. Evaporation left an oil which was purified by HPLC (20:1 dichloromethane-methanol) to give 2.95 g of 3-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)-2,2-dimethyl-propanoic acid a solid.

WORKUP

后处理

  1. temperaturethen heated
  2. temperatureto reflux for 5 hours
  3. customEvaporation
  4. waitleft an oil which
  5. customwas purified by HPLC (20:1 dichloromethane-methanol)