HRID1087381

反应详情

EQUATION

反应方程式

HRID 1087381 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the product from Step 2 (250 mg, 0.965 mmol) in tetrahydrofuran (THF, 4 mL) there was added 85% trimethylsilyl isocyanate (196 mg, 1.45 mmol) and the solution was stirred at room temperature for 1 hour. Water (4 mL) was added, stirring was continued for 10 minutes, then the THF was evaporated; the residue was extracted twice with ether and the crude product obtained from evaporation of the extracts was crystallized from ether to afford the title compound as white crystals, m.p.: dec 155° C. with gassing.

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued for 10 minutes
  3. customthe THF was evaporated
  4. extractionthe residue was extracted twice with ether
  5. customthe crude product obtained from evaporation of the extracts
  6. customwas crystallized from ether