HRID2406336

反应详情

EQUATION

反应方程式

HRID 2406336 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-(1-methanesulfonyl-1,2,3,6-tetrahydro-pyridin-4-yl)-dispiro[2,3-dihydrofuro[2,3-c]pyridine-2,1′-cyclobutane-3′,4″-piperidine] (HCl salt, 0.22 g) and N,N-diisopropyl-ethylamine (0.22 mL) in dichloromethane (20 mL) is stirred at room temperature for 5 min. Bromocyanide (60 mg) is added and the solution is stirred at room temperature for 2 h. Water is added and the mixture is extracted with dichloromethane. The combined extracts are dried (Na2SO4) and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate/methanol 5:5:0→5:4:1) to give the title compound. Mass spectrum (ESI+): m/z=415 [M+H]+.

WORKUP

后处理

  1. stirringthe solution is stirred at room temperature for 2 h
  2. extractionthe mixture is extracted with dichloromethane
  3. dry with materialThe combined extracts are dried (Na2SO4)
  4. concentrationconcentrated
  5. customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate/methanol 5:5:0→5:4:1)