HRID2254642

反应详情

EQUATION

反应方程式

HRID 2254642 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The procedure is as in Example 1, starting with 4-trifluoromethoxy-2-methylaniline (0.65 g), potassium thiocyanate (1.3 g) and bromine (0.35 cc) in acetic acid (12 cc). After purification on a column of silica (200 g; particle size: 0.063-0.200 mm), eluting with a cyclohexane/ethyl acetate mixture (50:50 by volume), the white solid obtained (0.65 g) is ground in cyclohexane (20 cc), drained and dried at 60° C. under reduced pressure (1 mm Hg; 0.13 kPa), to give 4-methyl-6-trifluoromethoxy-2-benzothiazolamine (0.6 g), m.p. 162° C.

WORKUP

后处理

  1. customAfter purification on a column of silica (200 g; particle size: 0.063-0.200 mm)
  2. washeluting with a cyclohexane/ethyl acetate mixture (50:50 by volume)
  3. customthe white solid obtained (0.65 g)
  4. customdried at 60° C. under reduced pressure (1 mm Hg; 0.13 kPa)