HRID542756

反应详情

EQUATION

反应方程式

HRID 542756 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 8-fluoro-11-(1-methyl-4-piperidylidene)-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridine (10.5 g, 34 mmol) and triethylamine (5.2 g, 52 mmol) in dry toluene (120 mL) at 80° C. under an argon atmosphere, was added ethylchloroformate (18.5 g, 170 mmol) via a syringe. The reaction mixture was allowed to stir at this temperature for 30 minutes and at room temperature for one hour. The reaction mixture was then filtered and solvent was removed. The residue was triturated with pentane to give 10.1 grams (yield=81%) of the title compound, m.p.=116°-118° C.

WORKUP

后处理

  1. filtrationThe reaction mixture was then filtered
  2. customsolvent was removed
  3. customThe residue was triturated with pentane