反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 110 °C
PROCEDURE
实验过程
A mixture of (5-bromo(2-thienyl)-N-(2,6-difluorophenyl)carboxamide (19 mg, 0.06 mmol), 5-chloro-6-(4,4,5,5-tetramethyl(1,3,2-dioxaborolan-2-yl))benzothiazole (20) (17 mg, 0.06 mmol), tetrakis(triphenylphosphine)-palladium(0) (Pd(Ph3P)4, 7 mg) and sodium carbonate (19 mg) in 0.5 ml DME, 0.5 ml EtOH and 0.25 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 silica gel flash chromatography (0-80% B; A: hexane; B: 50% EA in hexane) to furnish 17.8 mg of N-(2,6-difluorophenyl)[5-(5-chlorobenzothiazol-6-yl)(2-thienyl)]carboxamide (21) as white solid (yield: 72.9%; purity>95%). LC-MS: calcd. for C18H9F2ClN2OS2: 407 (M+1).
WORKUP
后处理
- concentrationphase was concentrated