HRID459607

反应详情

EQUATION

反应方程式

HRID 459607 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 5-amino-1-methyl-4-phenoxycarbonylaminopyrazole (153.8 g) in tetrahydrofuran (1 L) were added triethylamine (67 g) and triphenylmethyl chloride (185 g) at room temperature. The mixture was stirred for 6.5 hours. To the reaction mixture was added heptane (2.6 L) and the mixture was stirred for 1 hour. The precipitated solid was collected by filtration and washed with heptane-diisopropyl ether (1:1). The crude solid was suspended in water (3 L) and the suspension was stirred for 1 hour. The solid was collected by filtration and dried to give 1-methyl-4-phenoxycarbonylamino-5-triphenylmethylaminopyrazole (253.6 g).

WORKUP

后处理

  1. stirringthe mixture was stirred for 1 hour
  2. filtrationThe precipitated solid was collected by filtration
  3. washwashed with heptane-diisopropyl ether (1:1)
  4. stirringthe suspension was stirred for 1 hour
  5. filtrationThe solid was collected by filtration
  6. customdried