HRID469588

反应详情

EQUATION

反应方程式

HRID 469588 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of the above crude 2-diazo-1-(1-(trifluoromethyl)cyclopentyl)ethanone and the product from Example 86A in 1,2-dichloroethane and 1-methyl-2-pyrrolidinone was microwaved at 200° C. for 15 minutes, diluted with EtOAc, washed with saturated aqueous NaHCO3 and brine, dried (Na2SO4), and filtered. The residue was chromatographed on SiO2 (1-2% acetone/dichloromethane) to give the title compound as a white solid: 1H NMR (300 MHz, CDCl3) δ ppm 8.50-8.58 (m, 1H), 8.47-8.50 (bs, 1H), 7.78-7.86 (m, 2H), 7.67-7.75 (m, 1H), 7.52-7.57 (m, 2H), 7.48-7.52 (m, 2H), 2.67 (s, 2H), 2.07-2.18 (m, 2H), 1.94-2.04 (m, 2H), 1.67-1.84 (m, 4H); MS (ESI−) M/Z 448 (M−H)−.

WORKUP

后处理

  1. washwashed with saturated aqueous NaHCO3 and brine
  2. dry with materialdried (Na2SO4)
  3. filtrationfiltered
  4. customThe residue was chromatographed on SiO2 (1-2% acetone/dichloromethane)