反应详情

Acetyl chloride (6.5 g) is added dropwise to a stirring solution of the amine of step 4 above (5 g) in pyridine (80 ml) cooled in an ice bath. The reaction mixture is allowed to warm to RT with stirring for 45 minutes. Water is added, the mixture again cooled in ice, and partitioned between H2O and CH2Cl2. The organic layer is separated and washed successively with H2O, 10% HCl, aqueous saturated NaHCO3, dried, filtered and evaporated affording a solid residue which is recrystallized from Hexane-Ethyl acetate, M.P. 110°-112° C. NMR (90 MHz, DMSO-d6) shows the correct compound.

1. temperaturecooled in an ice bath
2. temperaturethe mixture again cooled in ice
3. custompartitioned between H2O and CH2Cl2
4. customThe organic layer is separated
5. washwashed successively with H2O, 10% HCl, aqueous saturated NaHCO3
6. customdried
7. filtrationfiltered
8. customevaporated
9. customaffording a solid residue which
10. customis recrystallized from Hexane-Ethyl acetate, M.P. 110°-112° C