HRID840267

反应详情

EQUATION

反应方程式

HRID 840267 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 1.0 gm (3.22 mmole) of 4-(8-chloro-5,6-dihydro-11H-benzo[5,6]cyclohepta[1,2-b]pyridin-11-ylidene) piperidine and 0.29 mL of pyridine in 20 mL of dry CH2Cl2 at 0° C. and under an argon atmosphere was added dropwise 0.438 mL (3.55 mmol) of 2-thiopheneacetyl chloride. After 30 minutes the mixture was washed with 1.0 N aqueous NaOH and then brine. The organic portion was dried over Na2SO4, filtered and converted in vacuo to provide a residue which was purified via flash chromatography (3% MeOH in CH2Cl2) and treated with activated carbon to provide the title compound as a glass.

WORKUP

后处理

  1. washAfter 30 minutes the mixture was washed with 1.0 N aqueous NaOH
  2. dry with materialThe organic portion was dried over Na2SO4
  3. filtrationfiltered
  4. customto provide a residue which
  5. customwas purified via flash chromatography (3% MeOH in CH2Cl2)
  6. additiontreated with activated carbon