HRID2095522

反应详情

EQUATION

反应方程式

HRID 2095522 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In analogy to intermediate 40B, 3,4-bis(trifluoromethyl)aniline and ethyl 2-bromopropionate with 2,6-lutidine were heated for 20 h at 82° C., diluted with acetonitrile and treated with 1 equivalent of ethyl 2-bromopropionate and 2,6-lutidine and refluxed for 2 days, treated again with 1 equivalent of ethyl 2-bromopropionate and 2,6-lutidine and continued to reflux for 2 days. Workup and purification by flash silica gel column (n-heptane/ethyl acetate 9:1 to 2:1) yielded 49% of the titled compound as yellow oil. MS: 328.08 (M−H−).

WORKUP

后处理

  1. temperaturerefluxed for 2 days
  2. temperatureto reflux for 2 days
  3. customWorkup and purification by flash silica gel column (n-heptane/ethyl acetate 9:1 to 2:1)