HRID449656

反应详情

EQUATION

反应方程式

HRID 449656 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

tert-Butyl (6-(6-chloro-2-methyl-3-oxo-2,3-dihydropyridazin-4-ylamino)pyridin-3-yl)methyl(2-methoxyethyl)carbamate (95 mg, 0.22 mmol) was dissolved in 0.75 ml of formic acid and 1.4 ml of formalin. The reaction was heated at 70° C. for 4 hours. The reaction was cooled to room temperature, water was added and the aqueous layer was extracted with DCM. The aqueous layer was carefully basified with solid potassium carbonate and extracted 3 times with DCM. The crude product was purified by chromatography using a gradient of 5% to 15% methanol in DCM to give 50 mg (66.0%) of a white powder.

WORKUP

后处理

  1. temperatureThe reaction was cooled to room temperature
  2. extractionthe aqueous layer was extracted with DCM
  3. extractionextracted 3 times with DCM
  4. customThe crude product was purified by chromatography