HRID391412

反应详情

EQUATION

反应方程式

HRID 391412 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

(3-(5-Methyl-1H-tetrazol-1-yl)-5-(trifluoromethyl)phenyl)methanol (110 mg, 0.46 mmol) and triphenylphosphine (240 mg, 0.93 mmol) were combined in methylene chloride (4 mL) and cooled to 0° C. N-Bromosuccinimide (171 mg, 0.96 mmol) was introduced in portions and the reaction allowed to warm to room temperature. After 16 h, the reaction mixture was diluted with ethyl acetate, washed with concentrated sodium bicarbonate (2×), brine (2×), dried over sodium sulfate, and concentrated. Column chromatography on silica gel (20% ethyl acetate/hexanes) gave 120 mg (82%). LC/MS (HPLC method 3): tR=2.30 min, 323.01 (MH)+.

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. washwashed with concentrated sodium bicarbonate (2×), brine (2×)
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. customColumn chromatography on silica gel (20% ethyl acetate/hexanes) gave 120 mg (82%)