HRID976644

反应详情

EQUATION

反应方程式

HRID 976644 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trifluoroacetic acid (42 mL, 544 mmole) was added to a chilled (0° C.) solution of tert-butyl N-benzyloxy-N-(1-ethylpropyl)carbamate (21.6 g, 73.6 mmole) in methylene chloride (300 mL). The reaction was stirred at ambient temperature for about 18 hours then concentrated under vacuum. Saturated aqueous sodium bicarbonate (100 mL) was added to the residue followed by a quantity of solid sodium carbonate sufficient to adjust the pH of the reaction mixture to pH 9. The reaction mixture was extracted with diethyl ether (4×50 mL). The extracts were combined, dried over sodium sulfate then concentrated to provide 10.9 g of N-benzyloxy-N-(1-ethylpropyl)amine as an oil.

WORKUP

后处理

  1. concentrationthen concentrated under vacuum
  2. additionSaturated aqueous sodium bicarbonate (100 mL) was added to the residue
  3. extractionThe reaction mixture was extracted with diethyl ether (4×50 mL)
  4. dry with materialdried over sodium sulfate
  5. concentrationthen concentrated