HRID518628

反应详情

EQUATION

反应方程式

HRID 518628 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of cis-4-(tert-butoxycarbonylamino)cyclohexanecarboxylic acid (3 g, 12.33 mmol) in DCM (35 mL) was added CDI (4.00 g, 24.66 mmol) portion-wise. The resulting mixture was stirred for 1 hour, and then O,N-dimethylhydroxylamine hydrochloride (1.804 g, 18.50 mmol) was added, and the mixture was stirred at RT for 16 hours. Water (30 mL) was added, and the mixture was stirred for 1 hour and then extracted with DCM (50 mL). The organic layer was washed with brine (30 mL), dried over sodium sulfate and concentrated to afford tert-butyl cis-4-(methoxy(methyl)carbamoyl)cyclohexylcarbamate (3.3 g, 93% yield).

WORKUP

后处理

  1. stirringthe mixture was stirred at RT for 16 hours
  2. stirringthe mixture was stirred for 1 hour
  3. extractionextracted with DCM (50 mL)
  4. washThe organic layer was washed with brine (30 mL)
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated