Hydrochloric Acid → 4-Morpholin-4-yl-3-(trifluoromethyl)benzoic acid
Reaktionsgleichung
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:14]=[CH:13][C:10]([C:11]#N)=[CH:9][C:8]=2[C:15]([F:18])([F:17])[F:16])[CH2:3][CH2:2]1.[OH-:19].[Na+].Cl.O1CCCC1.C[OH:28].O>>[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:14]=[CH:13][C:10]([C:11]([OH:28])=[O:19])=[CH:9][C:8]=2[C:15]([F:18])([F:17])[F:16])[CH2:3][CH2:2]1Komponenten
5
Versuchsvorschrift
4-Morpholino-3-(trifluoromethyl)benzonitrile (2.1 g, 8.016 mmol) was dissolved in a mixture of tetrahydrofurane/methanol/water (1:1:1, v/v/v, 20 mL), sodium hydroxide (1.9 g, 48.10 mmol) was added thereto and stirred for 40 hours with reflux. The reaction mixture was cooled to room temperature and 1N hydrochloride was added slowly thereto to pH 3˜4. The resulting solid was filtered, washed with water and dimethyl ether and then dried to obtain the title compound (694 mg).
Aufarbeitung
- additionwas added
- temperaturewith reflux
- filtrationThe resulting solid was filtered
- washwashed with water and dimethyl ether
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-858d4b4f6e35483d9c5f87124b0121d1
- Quelldatensatz
- uspto-grants-2015_04
- Patentnummer
- US08999973B2
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