HRID2096479

反应详情

EQUATION

反应方程式

HRID 2096479 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 6-bromo-2-(2-fluorophenyl)-1′-methyl-2′-(methylthio)spiro-[chroman-4,4′-imidazol]-5′(1′H)-one (80 mg, 0.183 mmol) and NH4I (53.21 mg, 0.367 mmol) in NH3/EtOH (2 mL, 1.5 N) was heated at 110° C. in a tube in a microwave reactor for 3 h. After cooling, the mixture was concentrated in vacuo to give a residue, which was purified by preparative TLC to afford 2′-amino-6-bromo-2-(2-fluorophenyl)-1′-methylspiro-[chroman-4,4′-imidazol]-5′(1′H)-one (52 mg, 70%). 1H-NMR (MeOD): 2.15 (d, 1H), 2.25 (d, 1H), 3.20 (s, 3H), 6.15 (d, 1H), 6.78 (d, 1H), 6.99 (t, 1H), 7.05 (s, 1H), 7.15 (t, 1H), 7.25 (d, 2H), 7.50 (t, 1H).

WORKUP

后处理

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