HRID12250

反应详情

EQUATION

反应方程式

HRID 12250 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The 3,3-dimethyl-4-oxo-piperidine-1-carboxylic acid tert-butyl ester thus prepared (450 mg, 1.97 mmol) was dissolved in methylene chloride (10 mL). Trifluoroacetic acid was added (305 uL) and the resulting solution stirred at room temperature 2 h. Additional trifluoroacetic acid was added (300 uL) and the reaction stirred at room temperature 3 days. The pale yellow solution was concentrated to afford an oily residue, which was triturated with ether. The solids were collected by suction filtration and dried in vacuo. 3,3-Dimethyl-piperidin-4-one was isolated and used as its trifluoroacetic acid salt (381 mg, 80%).

WORKUP

后处理

  1. stirringthe reaction stirred at room temperature 3 days
  2. concentrationThe pale yellow solution was concentrated
  3. customto afford an oily residue, which
  4. customwas triturated with ether
  5. filtrationThe solids were collected by suction filtration
  6. customdried in vacuo