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HRID2201987

反应详情

EQUATION

反应方程式

HRID 2201987 的结构方程式

REACTANTS

反应物

3
结构：CS(C)=O
HCID679

Dimethyl sulfoxide

C2H6OS

结构：CC(C)(C)N
HCID6385

tert-Butylamine

C4H11N

结构：C[C@@H]1CC[C@@H](Nc2nc(Cl)ncc2C(N)=O)C[C@H]1O
HCID118253788

未命名化合物

PRODUCTS

生成物

1
结构：C[C@@H]1CC[C@@H](Nc2nc(NC(C)(C)C)ncc2C(N)=O)C[C@H]1O
HCID71237511

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：O
溶剂HCID962

Water

H2O

CONDITIONS

反应条件

温度
68 °C

PROCEDURE

实验过程

A mixture of 2-chloro-4-((1R,3R,4R)-3-hydroxy-4-methylcyclohexylamino)pyrimidine-5-carboxamide (4 g), tert-butylamine (14 mL) and DMSO (20 mL) was heated to 68° C. and held for 60 hours. After cooling to room temperature, water (20× vol, 80 mL) was added over 2 hours. The slurry was agitated for 2 hours and the crude product was collected as the DMSO hemi-solvate of 2-(tert-butylamino)-4-((1R,3R,4R)-3-hydroxy-4-methylcyclohexylamino)-pyrimidine-5-carboxamide (Form H) by suction filtration.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. filtrationthe crude product was collected as the DMSO hemi-solvate of 2-(tert-butylamino)-4-((1R,3R,4R)-3-hydroxy-4-methylcyclohexylamino)-pyrimidine-5-carboxamide (Form H) by suction filtration