HRID1408590

反应详情

EQUATION

反应方程式

HRID 1408590 的结构方程式

PROCEDURE

实验过程

A solution of 6-bromo-2-(2,3-difluorophenyl)-1′-methyl-2′-(methylthio)spiro[chroman-4,4′-imidazol]-5′(1′H)-one (63 mg, 0.14 mmol), NH4I (60.6 mg, 0.42 mmol) in a solution of NH3/EtOH (3 mL, 1.5 N) was heated at 110° C. in a tube under microwave reactor for 3 hrs. After cooling, the mixture was concentrated in vacuo to give the residue, which was purified by preparative TLC to afford 2′-amino-6-bromo-2-(2,3-difluorophenyl)-1′-methylspiro[chroman-4,4′-imidazol]-5′(1′H)-one (35 mg, 60%). 1H-NMR (CDCl3): 2.31 (d, 1H), 2.45 (t, 1H), 3.27 (s, 3H), 6.12 (d, 1H), 6.87 (m, 1H), 7.09 (m, 3H), 7.34 (m, 2H), 7.45 (m, 1H).

WORKUP

后处理

  1. temperatureAfter cooling
  2. concentrationthe mixture was concentrated in vacuo
  3. customto give the residue, which
  4. customwas purified by preparative TLC