HRID1365270

反应详情

EQUATION

反应方程式

HRID 1365270 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 236 (1.0 eq) in acetonitrile (0.1M) at r.t. was added chlorosulfonyl isocyanate (10 eq) dropwise. The reaction was stirred for 40 minutes, then concentrated. To the residue was added 2N HCl and mixture was heated to 80° C. for 20 minutes. Reaction mixture was allowed to cool down to room temperature, and was neutralized with NaOH 6M. Mixture was then concentrated. The crude product was purified by reverse phase HPLC to give 6 mg of 247. MS (Q1) 517 (M+

WORKUP

后处理

  1. concentrationconcentrated
  2. additionTo the residue was added 2N HCl and mixture
  3. customReaction mixture
  4. temperatureto cool down to room temperature
  5. concentrationMixture was then concentrated
  6. customThe crude product was purified by reverse phase HPLC