HRID2406363

反应详情

EQUATION

反应方程式

HRID 2406363 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 5-(4-methylsulfanyl-phenyl)-1″-tert-butoxycarbonyl-dispiro[2,3-dihydrofuro[2,3-c]pyridine-2,1′-cyclobutane-3′,4″-piperidine] (100 mg), potassium cyanide (22 mg), copper(II) bromide (20 mg), palldium(II) acetate (5 mg), and N,N-dimethylformamide (5 mL) is stirred in air at 130° C. overnight. After cooling to room temperature, water is added and the mixture is extracted with ethyl acetate. The combined extract is dried (Na2SO4) and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate) to give the title compound. LC (method 3): tR=1.17 min; Mass spectrum (ESI+): m/z=478 [M+H]+.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. extractionthe mixture is extracted with ethyl acetate
  3. extractionThe combined extract
  4. dry with materialis dried (Na2SO4)
  5. concentrationconcentrated
  6. customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate)