Reaktionsgleichung
Br[CH2:2][C:3]1[CH:4]=[C:5]([CH:8]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=1)[C:6]#[N:7].[NH3:15].CO>>[NH2:15][CH2:2][C:3]1[CH:4]=[C:5]([CH:8]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=1)[C:6]#[N:7]Komponenten
3
Reaktionsbedingungen
- Temperatur
- 55 °C
Versuchsvorschrift
3-Bromomethyl-5-trifluoromethyl-benzonitrile (which is prepared in Reference Example 12) (15.9 g) is dissolved in 7M-ammonia/methanol (550 ml), and the mixture is stirred at 50-60° C. for 30 minutes. The reaction solution is concentrated under reduced pressure. To the resulting residue are added a saturated aqueous sodium bicarbonate solution and chloroform, and the mixture is separated, and the organic layer is dried over sodium sulfate, and concentrated under reduced pressure. The resulting residue is purified by silica gel column chromatography (chloroform:methanol=1:0→19:1→chloroform:methanol:ammonium hydroxide solution=19:1:0.1) to give 3-aminomethyl-5-trifluorometyl-benzonitrile (10.4 g). MS (m/z): 201 [M+H]+
Aufarbeitung
- concentrationThe reaction solution is concentrated under reduced pressure
- additionTo the resulting residue are added a saturated aqueous sodium bicarbonate solution and chloroform
- customthe mixture is separated
- dry with materialthe organic layer is dried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe resulting residue is purified by silica gel column chromatography (chloroform:methanol=1:0→19:1→chloroform:methanol:ammonium hydroxide solution=19:1:0.1)
Quellen und Nachweise
- ORD-Eintrag
- ord-59a4312b22d24405804e93c91807a522
- Quelldatensatz
- uspto-grants-2011_12
- Patentnummer
- US08076364B2
Verknüpfte Notizen
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