HRID74623

反应详情

EQUATION

反应方程式

HRID 74623 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

314 mg (1.08 mmol) 1-piperidin-4-yl-1,3-dihydroimidazo[4,5-b]pyridin-2-one dihydrochloride were added to 300 mg (1.08 mmol) (4-chloropyridin-2-yl)-(5-fluoro-2,3-dihydro-indol-1-yl)-methanone and 373 mg (2.70 mmol) potassium carbonate in 5.0 mL N-methylpyrrolidone. The reaction mixture was stirred for 30 h at 130° C. Then the mixture was poured onto 100 mL water and extracted with EtOAc (3×100 mL). The combined organic phases were dried and evaporated down using the rotary evaporator. The residue was purified by preparative HPLC. The product fractions were combined and evaporated down i. vac. The residue was triturated with 30 mL diethyl ether. The precipitated solid was suction filtered and dried in the air.

WORKUP

后处理

  1. extractionextracted with EtOAc (3×100 mL)
  2. customThe combined organic phases were dried
  3. customevaporated
  4. customthe rotary evaporator
  5. customThe residue was purified by preparative HPLC
  6. customevaporated down i
  7. customThe residue was triturated with 30 mL diethyl ether
  8. filtrationfiltered
  9. customdried in the air