反应详情

温度

10 °C

To a solution of 8.1 parts of 4-amino-5-chloro-2,3-dihydro-2,2-dimethyl-7-benzofurancarboxylic acid in 218 parts of Irichloromethane and 3.43 parts of N,N-diethyl-ethanamine were added dropwise 3.63 parts of ethyl chloroformate, keeping the temperature below 10° C. After stirring for 1/2 hour at 10° C., the whole was added to a solution of 6.26 parts of ethyl 4-amino-3-methoxy-1-piperidinecarboxylate in 145 parts of trichloromethane at 10° C. Stirring was continued for 1/2 hour at room temperature. The reaction mixture was washed with water, NaOH 5% and water and was then dried, filtered and evaporated. The residue was suspended in 2,2'-oxybispropane. The product was filtered off and dried, yielding 12.3 parts (93.2%) of ethyl cis-4-[(4-amino-5-chloro-2,3-dihydro-2,2-dimethyl-7-benzofuranyl)carbonylamino]-3-methoxyl-piperidinecarboxylate (interm. 1).

1. customthe temperature below 10° C
2. stirringStirring
3. waitwas continued for 1/2 hour at room temperature
4. washThe reaction mixture was washed with water, NaOH 5% and water
5. customwas then dried
6. filtrationfiltered
7. customevaporated
8. filtrationThe product was filtered off
9. customdried