HRID1715358

反应详情

EQUATION

反应方程式

HRID 1715358 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The titled compound was prepared from 1-(5-bromo-2-thienyl)-2,2,2-trifluoroethanone (C2) (1.0 eq) and the corresponding 4-carboxyphenylboronic acid (1.3 eq) in DMF (1.0M) following the general procedure for Suzuki cross-coupling described in example 3 step 1. After completation of the reaction the solution mixture was concentrated under reduced pressure and 1N HCl solution was added. The resulting precipitate formed was washed several times with DCM and used in the next coupling reaction without further purification. 1H NMR (400 MHz, DMSO, 300K) δ 13.14 (1H, broad s), 8.18 (1H, broad s), 8.06-8.00 (4H, m), 7.95 (1H, d, J=4.2 Hz). MS (ES) C13H7F3O3S requires: 300, found: 301 (M+H+).

WORKUP

后处理

  1. customAfter completation of the reaction the solution mixture
  2. concentrationwas concentrated under reduced pressure and 1N HCl solution
  3. additionwas added
  4. customThe resulting precipitate formed
  5. washwas washed several times with DCM
  6. customused in the next coupling reaction without further purification