反应详情

A mixture of 8.7 parts of 1-acetyl-N-(2-benzothiazolyl)-4-piperidinemethanamine, 1.44 parts of a sodium hydride dispersion 60% and 270 parts of N,N-dimethylformamide was stirred for 1 hour at room temperature. 5.48 Parts of iodomethane were added dropwise slowly. Upon completion, stirring was continued overnight at room temperature. The reaction mixture was poured into water. The product was extracted with 4-methyl-2-pentanone. The extract was dried, filtered and evaporated in vacuo. The residue was purified by column chromatography (HPLC) over silica gel using a mixture of dichloromethane and methanol (98.75:1.25 by volume) as eluent. The second fraction was collected and the eluent was evaporated, yielding 7.6 parts (84%) of 1-acetyl-N-(2-benzothiazolyl)-N-methyl-4-piperidinemethanamine as a residue (intermediate 52).

1. stirringUpon completion, stirring
2. waitwas continued overnight at room temperature
3. extractionThe product was extracted with 4-methyl-2-pentanone
4. customThe extract was dried
5. filtrationfiltered
6. customevaporated in vacuo
7. customThe residue was purified by column chromatography (HPLC) over silica gel using
8. additiona mixture of dichloromethane and methanol (98.75:1.25 by volume) as eluent
9. customThe second fraction was collected
10. customthe eluent was evaporated