反应 #40674

反应方程式

Ethyl isonipecotate

triethyl amine

Trimethylacetyl chloride

→

20a

收率 94.0%

Ethyl 1-pivaloylpiperidine-4-carboxylate

收率 94.0%

溶剂

dichloromethane

反应条件

后处理

1. 1
   温度to warm to rt
2. 2
   洗涤The reaction mixture was washed with hydrochloric acid solution (1.0 M, aq), sodium bicarbonate (sat., aq.) and sodium chloride (sat., aq.)
3. 3
   干燥The organic layer dried over magnesium sulfate
4. 4
   过滤filtered
5. 5
   其他the solvent removed

实验过程

Ethyl isonipecotate (20 mL, 130 mmol) was dissolved in 130 mL of dichloromethane and cooled to 0° C. and triethyl amine (19.9 mL, 143 mmol) was added. Trimethylacetyl chloride (16.8 mL, 136 mmol) was added dropwise and the reaction was allowed to warm to rt and stirred for 16 h. The reaction mixture was washed with hydrochloric acid solution (1.0 M, aq), sodium bicarbonate (sat., aq.) and sodium chloride (sat., aq.). The organic layer dried over magnesium sulfate, filtered and the solvent removed to provide 29.5 g (94%) of 20a as a pale orange liquid. LC-MS m/z 242 [M+H]+.

来源