HRID74548

反应详情

EQUATION

反应方程式

HRID 74548 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.50 g (3.2 mmol) 4-chloropicolinic acid, 1.1 g (3.4 mmol) TBTU and 0.91 mL (6.5 mmol) TEA were placed in 10 mL DMF. 0.63 g (3.3 mmol) 4,5-difluoroindoline hydrochloride were added. The reaction mixture was stirred overnight at RT and then extracted successively with a 15% potassium carbonate solution, water, a 1M HCl solution and EtOAc. The organic phase was dried, filtered and concentrated to dryness by rotary evaporation. The residue was stirred with diisopropylether and the undissolved solid was suction filtered and dried.

WORKUP

后处理

  1. extractionextracted successively with a 15% potassium carbonate solution, water
  2. customThe organic phase was dried
  3. filtrationfiltered
  4. concentrationconcentrated to dryness by rotary evaporation
  5. stirringThe residue was stirred with diisopropylether
  6. filtrationfiltered
  7. customdried