HRID548782

反应详情

EQUATION

反应方程式

HRID 548782 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Ethoxycarbonyl isothiocyanate (0.144 g, 1.1 mmol) was added to a stirred solution of 4-[(2-methoxy-2-methylpropyl)amino]-1H-imidazole-5-carboxamide (0.155 g, 0.73 mmol), which was obtained from Example 3(b), in CH2Cl2 (2.5 mL) at r.t. for 16 h. The solvent was evaporated and the residue was then dissolved in 2% aqueous sodium hydroxide (NaOH) solution (10 mL) and heated at 50° C. for 3 h. The pH was adjusted to neutral with 2 M HCl and the resulted precipitates were collected by filtration followed by prep-HPLC purification. The title compound was obtained as a white solid in 32% yield (60 mg).

WORKUP

后处理

  1. customThe solvent was evaporated
  2. dissolutionthe residue was then dissolved in 2% aqueous sodium hydroxide (NaOH) solution (10 mL)
  3. customthe resulted precipitates
  4. filtrationwere collected by filtration
  5. customfollowed by prep-HPLC purification