تفاعل #40674

معادلة التفاعل

Ethyl isonipecotate

triethyl amine

Trimethylacetyl chloride

→

20a

المردود 94.0%

Ethyl 1-pivaloylpiperidine-4-carboxylate

المردود 94.0%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto warm to rt
2. 2
   غسيلThe reaction mixture was washed with hydrochloric acid solution (1.0 M, aq), sodium bicarbonate (sat., aq.) and sodium chloride (sat., aq.)
3. 3
   تجفيفThe organic layer dried over magnesium sulfate
4. 4
   ترشيحfiltered
5. 5
   أخرىthe solvent removed

الإجراء التجريبي

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]+.

المصدر