HRID2196737

反应详情

EQUATION

反应方程式

HRID 2196737 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

NaOH (1M, 3.20 mL, 3.20 mmol) was added to methyl 2,6-difluoro-3-(N-propylsulfamoylamino)benzoate (0.24 g, 0.80 mmol) in 2:1 THF:MeOH (3 mL). The solution was stirred at room temperature for 16 hours, and then the solution was stirred at 70° C. for 16 hours. The solution was concentrated under reduced pressure to about half volume and then washed with EtOAc. The pH was adjusted to about 5 and extracted with EtOAc (3×5 mL). The organic layers were dried over sodium sulfate, decanted and concentrated to provide 2,6-difluoro-3-(N-propylsulfamoylamino)benzoic acid.

WORKUP

后处理

  1. stirringthe solution was stirred at 70° C. for 16 hours
  2. concentrationThe solution was concentrated under reduced pressure to about half volume
  3. washwashed with EtOAc
  4. extractionextracted with EtOAc (3×5 mL)
  5. dry with materialThe organic layers were dried over sodium sulfate
  6. customdecanted
  7. concentrationconcentrated