HRID985438

反应详情

EQUATION

反应方程式

HRID 985438 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To toluene-4-sulfonic acid 5-[(S)-1-hydroxyethyl]-1H-pyrazol-3-yl ester (6.09 g, 21.6 mmol) in anhydrous dichloromethane (180 ml) was added pyridinium dichromate (9.74 g, 25.9 mmol) and the resulting slurry was stirred at room temperature for 17.6 h. The mixture was poured directly onto a column of silica gel, which was eluted with ethyl acetate to yield 5.13 g (85%) of the title compound as a whitish solid: 1H NMR (360 MHz, DMSO-d6) δ 2.43 (3H, s), 2.45 (3H, s), 6.78 (1H, s), 7.49 (2H, d, J=8.2 Hz), 7.80 (2H, d, J=8.3 Hz), 13.72 (1H, s); MS (ES+) m/e 281 [M+H]+.

WORKUP

后处理

  1. additionThe mixture was poured directly onto a column of silica gel, which
  2. washwas eluted with ethyl acetate