HRID1917065

反应详情

EQUATION

反应方程式

HRID 1917065 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of compound 9 (20.0 mg) in 10 mL CH2Cl2 was treated with 1.1 eq. of BF3—OEt2 under Ar. The mixture was stirred overnight and washed with 1N HCl and sat. NaHCO3 Removal of the solvent gave the crude product and TLC analysis showed one major spot. The crude product was further purified on SiO2 column to provide the title compound (16 mg). The structure was confirmed by NMR and TLC comparison with authentic sample prepared by the reaction of 7-MeO-2,3,4,5-tetrahydro-1,4-benzothiazepine with methyl chloroformate.

WORKUP

后处理

  1. washwashed with 1N HCl and sat. NaHCO3 Removal of the solvent
  2. customgave the crude product and TLC analysis
  3. customThe crude product was further purified on SiO2 column