HRID556387

反应详情

EQUATION

反应方程式

HRID 556387 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ice-cooled solution of H-Hse-OH (5 g) in dioxane/2M NaOH (168 mL/42 mL) was added benzyl chloroformate (6.7 mL) dropwise over 15 min. The reaction mixture was allowed to warm to RT and was stirred overnight at RT. The solvent was evaporated off and the aq. residue was extracted with Et2O and acidified with a 2M HCl solution. The aq. phase was extracted with DCM. The DCM layers were combined, washed with water, dried (Na2SO4) and evaporated off to give the desired product as a white powder (6.2 g).

WORKUP

后处理

  1. customThe solvent was evaporated off
  2. extractionthe aq. residue was extracted with Et2O
  3. extractionThe aq. phase was extracted with DCM
  4. washwashed with water
  5. dry with materialdried (Na2SO4)
  6. customevaporated off