反应详情

To a solution of 2M methylamine in MeOH (30 mL) was added intermediate 32 (2.91 g, 9.1 mmol, 1 eq). After stirring this mixture at room temperature for 30 min, the solvent was removed and the residue was partitioned between saturated NaHCO3 and DCM (2×100 mL). The organic layer was dried (Na2SO4) and concentrated. The resultant residue was dissolved in MeOH (25 mL) and, after addition of sodium borohydride (1.0 g, 27.6 mmol, 3 eq), the mixture was stirred at room temperature for 1 h. Solvent was removed and the residue was partitioned between a Na2CO3 solution and CHCl3. The resultant organic layer was dried (Na2SO4) and concentrated in vacuo to give 2.7 g, (88%) of (4-(4-methoxybenzyloxy)-3-bromophenyl)-N-methylmethanamine (33).

1. customthe solvent was removed
2. customthe residue was partitioned between saturated NaHCO3 and DCM (2×100 mL)
3. dry with materialThe organic layer was dried (Na2SO4)
4. concentrationconcentrated
5. dissolutionThe resultant residue was dissolved in MeOH (25 mL)
6. stirringthe mixture was stirred at room temperature for 1 h
7. customSolvent was removed
8. customthe residue was partitioned between a Na2CO3 solution and CHCl3
9. dry with materialThe resultant organic layer was dried (Na2SO4)
10. concentrationconcentrated in vacuo