HRID1830147

反应详情

EQUATION

反应方程式

HRID 1830147 的结构方程式

PROCEDURE

实验过程

A solution of {1-[hydroxy-(N-hydroxycarbamimidoyl)-methyl]-propyl}-carbamic acid tert-butyl ester (2) (2.5 g, 10 mmol) in dichloromethyl (125 ml) was treated with benzoic acid (1.36 g, 11 mmol), EDCI (2.14 g, 11 mmol), HOBT (1.37 g, 10 mmol) and triethylamine (1.35 ml, 11 mmol) and stirred at room temperature overnight. Reaction mixture was washed with saturated sodium bicarbonate solution and then water and dried over Na2SO4. Solvent evaporated under reduced pressure, crude purified by mplc eluting with 1% triethylamine in 2:3 v/v ethyl acetate and heptane mixture to give yellow solid (850 mg); MS: MH+ 352.

WORKUP

后处理

  1. customReaction mixture
  2. washwas washed with saturated sodium bicarbonate solution
  3. dry with materialwater and dried over Na2SO4
  4. customSolvent evaporated under reduced pressure, crude
  5. custompurified
  6. washby mplc eluting with 1% triethylamine in 2:3 v/v ethyl acetate and heptane mixture