4-Methylmorpholine → HCID 54574756, Verbindung

3-(3,4-Dichloro-phenyl)-3-(2-hydroxy-ethyl)-pyrrolidine (2 g, 7.695 mmol) was dissolved in dichloromethane at -78° C. and treated with 4-methylmorpholine (1.8 mL, 16.4 mmol, 2.1 eq.) and 2,6-dimethoxy-benzoyl chloride (1.55 g, 7.73 mmol) in dichloromethane (20 mL). The solution was allowed to warm to 0° C. and stirred for 1.5 hours. The solution was washed with 1N HCl and 5% sodium bicarbonate and the organic phase was dried over magnesium sulfate, filtered, and concentrated in vacuo. The residue was chromatographed on silica gel (200 g) with a gradient of 50% ethyl acetate in hexane to 6% methanol in dichloromethane to give 2.434 g (75%) of the title compound.

1. washThe solution was washed with 1N HCl and 5% sodium bicarbonate
2. dry with materialthe organic phase was dried over magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe residue was chromatographed on silica gel (200 g) with a gradient of 50% ethyl acetate in hexane to 6% methanol in dichloromethane

ORD-Eintrag

ord-7810e23a4ab24d9897590089f47c6a96

Quelldatensatz

uspto-grants-1997_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05635510