3-[BIS-(ETHOXYCARBONYLAMINO)-METHYL]-PYRIDINE synthesis
- Product Name:3-[BIS-(ETHOXYCARBONYLAMINO)-METHYL]-PYRIDINE
- CAS Number:2744-17-4
- Molecular formula:C12H17N3O4
- Molecular Weight:267.28
Yield:2744-17-4 88%
Reaction Conditions:
with toluene-4-sulfonic acid in benzene;Dean-Stark;Reflux;
Steps:
2 Diethyl (pyridin-3-ylmethylene)dicarbamate
p-Toluenesulfonic acid (5.00 g, 26.3 mmol) was added to a solution of ethyl carbamate (33.27 g, 373.4 mmol) and nicotinaldehyde (17.53 mL, 186.7 mmol) in benzene (400 mL). The solution was stirred at strong reflux with a Dean Stark apparatus (overnight). A precipitate formed during the reaction. The reaction mixture was cooled to 0°C and the material was filtrated. It was further washed twice with diethyl ether to afford a colorless solid (6.2 g, 88%).
References:
WO2021/260029,2021,A1 Location in patent:Page/Page column 55; 62; 80