HRID1524238

反应详情

EQUATION

反应方程式

HRID 1524238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of N-(5-bromo(1,3-thiazol-2-yl))(2,6-difluorophenyl)carboxamide (31 mg, 0.1 mmol), 6-methyl-5-(4,4,5,5-tetramethyl(1,3,2-dioxaborolan-2-yl))benzothiazole (14) (27 mg, 0.1 mmol), tetrakis(triphenylphosphine)-palladium(0) (Pd(Ph3P)4, 12 mg) and sodium carbonate (32 mg) in 0.5 ml DME, 0.5 ml EtOH and 0.2 ml water was heated under Ar in microwave reactor at 110° C. for 30 min. The reaction mixture was worked up with EA/brine. Org. phase was concentrated and then subjected to prep HPLC purification to give 4.6 mg (2,6-difluorophenyl)-N-[5-(6-methylbenzoxazol-5-yl)(1,3-thiazol-2-yl)]carboxamide (50) as pale brown solid (yield: 11.9%; purity>90%). LC-MS: calcd. for C18H11F2N3OS2: 388 (M+1).

WORKUP

后处理

  1. concentrationphase was concentrated
  2. customHPLC purification