HRID2076128

反应详情

EQUATION

反应方程式

HRID 2076128 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 3-methoxy-4-(2-methyl-thiazol-5-yl)-phenylamine (100 mg, 0.45 mmol) in tetrahydrofurane (4 mL) was added drop wise under stirring and under an atmosphere benzoyl isothiocyanate (67.7 ul, 0.48 mmol). The reaction was stirred at room temperature for 3 hours and the solvent was removed under reduced pressure. The residue was dissolved in methanol (6 mL) and a solution of potassium carbonate (188 mg, 1.36 mmol) in water (3 mL) was added. The resulting suspension was stirred at room temperature over night. The precipitate was filtered off, washed with water and diethyl ether to yield the title compound as a pale yellow solid (113 mg, 89%). MS ISP (m/e): 280.1 (100%) [(M+H)+]. 1H NMR (DMSO-D6, 300 MHz): δ (ppm)=9.82 (s, 1H, NH), 8.02 (s, 1H), 7.62 (d, 1H), 7.40 (s, 1H), 7.01 (s, 1H), 3.87 (s, 3H), 2.64 (s, 3H).

WORKUP

后处理

  1. customthe solvent was removed under reduced pressure
  2. dissolutionThe residue was dissolved in methanol (6 mL)
  3. stirringThe resulting suspension was stirred at room temperature over night
  4. filtrationThe precipitate was filtered off
  5. washwashed with water and diethyl ether