HRID711420

反应详情

EQUATION

反应方程式

HRID 711420 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of methyl 2-chloro-4-methyl-6-(m-tolylamino)pyrimidine-5-carboxylate (1.2 g, 4.11 mmol), tert-butyl (1S,2R)-2-aminocyclohexylcarbamate (0.882 g, 4.11 mmol) and triethylamine (1.720 mL, 12.34 mmol) in DMA (10 mL) was heated at 90° C. for 4 h. The solution was then diluted with EtOAc, washed with brine and water. The organic extract was dried and concentrated under reduced pressure to give a light yellow residue; white crystals were formed upon triturating with ACN (5 mL). The resultant solid was filtered, washed with ACN, and dried to give the title compound as white solid (1.2 g, 62%). [M+H] calc'd for C25H35N5O4, 470. found, 470.

WORKUP

后处理

  1. washwashed with brine and water
  2. extractionThe organic extract
  3. customwas dried
  4. concentrationconcentrated under reduced pressure
  5. customto give a light yellow residue
  6. customwhite crystals were formed
  7. customupon triturating with ACN (5 mL)
  8. filtrationThe resultant solid was filtered
  9. washwashed with ACN
  10. customdried