Hydrochloric Acid → 4-Morpholin-4-yl-3-(trifluoromethyl)benzoic acid

HRID 1465023Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1465023
[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]1

Komponenten

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

  1. additionwas added
  2. temperaturewith reflux
  3. filtrationThe resulting solid was filtered
  4. washwashed with water and dimethyl ether
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-858d4b4f6e35483d9c5f87124b0121d1
Quelldatensatz
uspto-grants-2015_04
Patentnummer
US08999973B2

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