反应详情

A solution of the product from Step 1 (500 mg, 1.94 mmol) in dichloromethane (5 ml) was cooled to 0° C. and treated with trifluoroacetic acid (2 ml). The mixture was allowed to warm to room temperature and stirred for a further 1 hour. After evaporation of the solvent in vacuo, the residue was partitioned between dichloromethane and an aqueous solution of sodium carbonate. After separation of the layers the aqueous phase was re-extracted six times with dichloromethane, dried and concentrated in vacuo to yield the title compound (145 mg, 47%); 1H NMR (CD3OD) 3.49 (2H, t, J 5.2 Hz), 3.35 (3H, s), 3.30 (2H, m), 3.10 (1H, s), 2.80 (2H, t, J 5.2 Hz), 2.68 (2H, m), 1.91 (2H, m), 1.30 (2H, m).

1. customAfter evaporation of the solvent in vacuo
2. customthe residue was partitioned between dichloromethane
3. customAfter separation of the layers the aqueous phase
4. extractionwas re-extracted six times with dichloromethane
5. customdried
6. concentrationconcentrated in vacuo