Potassium Carbonate → [4-(3,4-Dichlorobenzyl)morpholin-2-yl]methylamine

To a stirred solution of Intermediate 2 (2.97 g) in methanol (15 ml) and water (5 ml) was added potassium carbonate (5.53 g). The mixture was stirred at 22° C. for 18 h before the methanol was removed in vacuo. Water (25 ml) was added and the mixture extracted with ethyl acetate (3×30 ml). The combined organic phases were washed with water (5 ml) and saturated aqueous sodium chloride solution (10 ml) before drying over sodium sulphate, filtering and evaporation of the solvent in vacuo to give a pale yellow oil. The oil was purified by Biotage flash chromatography on a 90 g silica cartridge eluting with 75:8:1 dichloromethane/ethanol/0.880 ammonia solution. The required fractions were combined and the solvent evaporated in vacuo to give the title compound as a colourless oil (1.85 g).

1. customwas removed in vacuo
2. additionWater (25 ml) was added
3. extractionthe mixture extracted with ethyl acetate (3×30 ml)
4. washThe combined organic phases were washed with water (5 ml) and saturated aqueous sodium chloride solution (10 ml)
5. dry with materialbefore drying over sodium sulphate
6. filtrationfiltering
7. customevaporation of the solvent in vacuo
8. customto give a pale yellow oil
9. customThe oil was purified by Biotage flash chromatography on a 90 g silica cartridge
10. washeluting with 75:8:1 dichloromethane/ethanol/0.880 ammonia solution
11. customthe solvent evaporated in vacuo

ORD-Eintrag

ord-0b18c9ffa27c49ee8b442d891da4202c

Quelldatensatz

uspto-grants-2007_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07157457B2