HRID976626

反应详情

EQUATION

反应方程式

HRID 976626 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trifluoroacetic acid (21 mL, 270 mmol) was added in a single portion to a solution of tert-butyl N-benzyloxy-N-(2-methylpropyl)carbamate (7.6 g, 27 mmol) in methylene chloride (21 mL). A spontaneous reflux occurred. The reaction mixture was stirred without external heating for 20 minutes and then concentrated under vacuum at 45° C. Saturated aqueous sodium bicarbonate was added to the residue followed by a quantity of solid sodium bicarbonate sufficient to bring the pH of the reaction mixture up to a value of 9. The mixture was extracted twice with methylene chloride. The extracts were combined, dried over magnesium sulfate then concentrated under vacuum to provide 4.9 g of N-benzyloxy-N-(2-methylpropyl)amine as an oil.

WORKUP

后处理

  1. temperatureA spontaneous reflux
  2. temperaturewithout external heating for 20 minutes
  3. concentrationconcentrated under vacuum at 45° C
  4. additionSaturated aqueous sodium bicarbonate was added to the residue
  5. extractionThe mixture was extracted twice with methylene chloride
  6. dry with materialdried over magnesium sulfate
  7. concentrationthen concentrated under vacuum