HRID660536

反应详情

EQUATION

反应方程式

HRID 660536 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 5-[4-(3-aminopropyl)-2-benzyloxyphenyl]-1,1-dioxo-2-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-3-one TFA salt (124 mg, 0.26 mmol) in methylene chloride (5 mL) is added diisopropylethylamine (0.1 mg, 0.781 mmol) then acetyl chloride (21 mg, 0.267 mmol) and the mixture is stirred at RT for 18 h. The solvent is removed under reduced pressure and 1 N HCl is added. The mixture is extracted with ether and the organic phase is dried over magnesium sulfate. The solvent is removed under reduced pressure and the residue is purified by flash chromatography using a gradient of 10-50% EtOAc/hexane as eluent to give the title compound.

WORKUP

后处理

  1. customThe solvent is removed under reduced pressure and 1 N HCl
  2. additionis added
  3. extractionThe mixture is extracted with ether
  4. dry with materialthe organic phase is dried over magnesium sulfate
  5. customThe solvent is removed under reduced pressure
  6. customthe residue is purified by flash chromatography