HRID620573

反应详情

EQUATION

反应方程式

HRID 620573 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(RS)-Amino-1,3-dihydro-5-(2'-fluorophenyl)-2H-1,4-benzodiazepin-2-one (50 mg, 0.186 mmol) was suspended in methylene chloride (1 ml). Cinnamoyl chloride (34.5 mg, 0.207 mol) was added to the methylene chloride mixture. The pH of the stirred mixture was adjusted to ~9 with 50 μl of triethylamine. After stirring for 16 hours the mixture was filtered. The product in the filtrate was purified by prep TLC. The product band was collected by washing the silica containing the product, with 80:20:2 CMW. The solvent was evaporated and the residue was dissolved in methanol, placed in a small vial and evaporated. Yield 16.6 mg.

WORKUP

后处理

  1. filtrationwas filtered
  2. customThe product in the filtrate was purified by prep TLC
  3. customThe product band was collected
  4. washby washing the silica containing the product
  5. customThe solvent was evaporated
  6. dissolutionthe residue was dissolved in methanol
  7. customevaporated