HRID426276

反应详情

EQUATION

反应方程式

HRID 426276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 3-[5-isopropenyl-2,6-bis-(2-trimethylsilanyl-ethoxy)-pyrimidine-4-carbonyl]-5-methyl-benzonitrile (0.636 g, 1.28 mmol) in dichloromethane (10 mL) at 0° C. was added TFA (2 mL). Reaction mixture was stirred at 0° C. for 30 min, concentrated and purified by flash column chromatography (silica gel, 0 to 10% methanol/dichloromethane) to give a yellow solid (0.311 g, 82%). 1H NMR (300 MHz, CD3OD): δ 8.11 (s, 1H), 8.03 (s, 1H), 7.88 (s, 1H), 4.91 (s, 1H), 4.75 (s, 1H), 2.49 (s, 3H), 1.82 (s, 3H). Mass spectrum: 296.1 (M+H)+.

WORKUP

后处理

  1. customReaction mixture
  2. concentrationconcentrated
  3. custompurified by flash column chromatography (silica gel, 0 to 10% methanol/dichloromethane)