Hydrochloric Acid → HCID 22732530, Verbindung

A mixture of 4-(6-chloro-2-phenyl-4-pyrimidyl)morpholine (50 mg, 0.181 mmol), m-anisidine (20 μl, 0.181 mmol) and aqueous 2N HCl (150 μl) in water:ethanol (1:1, 10 ml) was refluxed for 5 days. The mixture was cooled to room temperature and basified with aqueous 2N NaOH to pH 10-12. The mixture was extracted with ethyl acetate (50 ml), which was washed with water (2×25 ml), aqueous saturated NaCl, and dried over anhydrous sodium sulfate. The ethyl acetate solution was concentrated in vacuo and isolated as a yellow solid (6 mg, 9%). 1H NMR (CDCl3): 8.40-8.37 (m, 2H), 7.46-7.43 (m, 3H), 7.31-7.25 (m, 2H), 7.00 (t, J=2.3 Hz, 1H), 6.91 (dd, J=1.7, 8.0 Hz, 1H), 6.70-6.67 (m, 2H), 3.83 (s, 3H), 3.81-3.63 (m, 8H).

1. temperaturewas refluxed for 5 days
2. extractionThe mixture was extracted with ethyl acetate (50 ml), which
3. washwas washed with water (2×25 ml), aqueous saturated NaCl
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationThe ethyl acetate solution was concentrated in vacuo

ORD-Eintrag

ord-f65e567069574c29881ff05bf7768602

Quelldatensatz

uspto-grants-2004_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06716851B2