HRID1914563

反应详情

EQUATION

反应方程式

HRID 1914563 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

5-Bromo-thiophene-3-carboxylic acid methyl ester (0.3 g, 1.35 mmol) was dissolved in toluene (5 mL), 2-tributylstannyl oxazole (0.311 mL, 1.48 mmol) was added then the reaction mixture was purged with nitrogen before addition of palladium tetrakis(triphenylphosphine) (0.14 g, 0.12 mmol). The reaction mixture was heated at 100° C. over the weekend. The mixture was filtered then evaporated and the residue was purified by chromatography on a silica II cartridge, eluting with 10-20% DCM in pentane to give the title compound as a yellow solid (0.105 g). LCMS m/z 210 [M+H]+ and 251.23 [M+MeCN+H]+ R.T.=3.03 min (Analytical Method 6).

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. customthen evaporated
  3. customthe residue was purified by chromatography on a silica II cartridge
  4. washeluting with 10-20% DCM in pentane