HRID632579

反应详情

EQUATION

反应方程式

HRID 632579 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 4-(bromomethyl)-benzaldehyde (0.940 g, 4.72 mmol) in dichloroethane (20 mL) was added L-leucine cyclopentyl ester tosylate (2.40 g, 6.4 mmol) and sodium triacetoxyborohydride (2.53 g, 11.9 mmol). The reaction mixture was stirred for 1 hour then poured into ethyl acetate (300 mL). The organic fraction was washed with saturated sodium hydrogen carbonate (100 mL, 3 times 50 mL) then dried (MgSO4), concentrated and purified by flash column chromatography (SiO2, gradient 0-3% methanol-dichloromethane) to yield the desired product (1.504 g, 83% yield). LC/MS: m/z 382/384 [M+H]+

WORKUP

后处理

  1. washThe organic fraction was washed with saturated sodium hydrogen carbonate (100 mL, 3 times 50 mL)
  2. dry with materialthen dried (MgSO4)
  3. concentrationconcentrated
  4. custompurified by flash column chromatography (SiO2, gradient 0-3% methanol-dichloromethane)