HRID1432075

反应详情

EQUATION

反应方程式

HRID 1432075 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of tert-butyl methylthiocarbonoimidoylcarbamate (Preparation AU, 0.98 g, 5.16 mmol), 3-(4-methoxyphenyl)-5-methyl-4-isoxazolecarboxylic acid (Preparation Y, 1.17 g, 5 mmol), EDCI (1.2 g, 6.26 mmol) and DIPEA (1 g, 7.75 mmol) in DCM (30 mL) was stirred for 3 hours. The solvent was concentrated by rotovap and residue was purified by column with EtOAc/DCM (5/95) as the eluant. The product was obtained as a white solid (1.2 g, 60%). 1H NMR (CD3OD): δ 1.52 (s, 9H), 1.89 (s, 3H), 2.76 (s, 3H), 3.86(s, 3H), 7.00,7.02 (d, 2H), 7.47,7.49 (d, 2H). MH+=406.19

WORKUP

后处理

  1. concentrationThe solvent was concentrated by rotovap and residue
  2. customwas purified by column with EtOAc/DCM (5/95) as the eluant