反应详情

To an ice-cooled solution of (R)-2-amino-8-(4-methylpiperazin-1-yl)-1,2,3,4-tetrahydronaphthalene (120 mg, 0.49 mmol), pyridine (100 μL, 1.2 mmol) and 4-dimethylaminopyridine (20 mg, 0.16 mmol) in methylene chloride (10 mL) was added dropwise trifluoroacetic anhydride (72 μL, 0.51 mmol). After the addition the reaction was allowed to stir at ambient temperature for 1 h and was then washed with water. The methylene chloride phase was dried (Na2SO4), filtered and evaporated in vacuo. The residue was purified on a silica gel column using ethyl acetate/methanol/concentrated ammonium hydroxide (96:4:0.5) as the eluent. This gave after crystallization from diethyl ether/hexane 41 mg (24% yield) of the title compound as white crystals: mp 158-159° C.; [α]21D +39° (c 0.25, chloroform); EIMS (70 eV) m/z (relative intensity) 341 (82, M+).

1. additionAfter the addition the reaction
2. washwas then washed with water
3. dry with materialThe methylene chloride phase was dried (Na2SO4)
4. filtrationfiltered
5. customevaporated in vacuo
6. customThe residue was purified on a silica gel column
7. customThis gave