反应详情

To a solution of the product of the above (2) (2.17 g) in absolute methanol (10 ml) is added a 30% solution (2.2 ml) of methylamine in methanol. The mixture is stirred at room temperature for 1 hour. Sodium borohydride (380 mg) is added to the filtrate. The mixture is stirred at room temperature for 2 hours and evaporated to remove the solvent. The residue is acidified with 2 N hydrochloric acid after addition of water. The solution is extracted with chloroform to remove neutral impurities. The aqueous layer is made alkaline with an aqueous solution of sodium hydroxide and extracted again with chloroform. The extract is washed with water, dried and evaporated to remove the solvent. The residue is treated with small amount of benzene to give the 1/6 benzene adduct (2.21 g) of the title compound melting at 78°-81° C. Yield: 90%

1. stirringThe mixture is stirred at room temperature for 2 hours
2. customevaporated
3. customto remove the solvent
4. additionafter addition of water
5. extractionThe solution is extracted with chloroform
6. customto remove neutral impurities
7. extractionextracted again with chloroform
8. washThe extract is washed with water
9. customdried
10. customevaporated
11. customto remove the solvent
12. additionThe residue is treated with small amount of benzene