Isobutyraldehyde → Benzyl(2-methylpropyl)amine
반응식
[CH:1](=O)[CH:2]([CH3:4])[CH3:3].[CH2:6]([NH2:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.P(O)(O)O>O>[CH2:6]([NH:13][CH2:1][CH:2]([CH3:4])[CH3:3])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1참가 물질
5
실험 절차
To the imine from isobutyraldehyde and benzylamine (48.4 g; 0.3 mole) was added phosphorous acid (24.6 g; 0.3 mole) and the mixture slowly warmed while stirring. As the internal temperature reached 70°-75° a vigorous exothermic reaction ensued taking the temperature to 130°-135°. After maintaining at 130°-140° for 30 mins. the viscous product was cooled to 100° and diluted with water. Basification and extraction with chloroform gave crude amine after solvent evaporation. Distillation gave pure N-benzylisobutylamine, 13.6 g (28%) bp 94°-99°/5.6 mm. Nmr confirmed the assigned structure.
후처리
- temperaturethe mixture slowly warmed
- customreached 70°-75°
- customa vigorous exothermic reaction
- customto 130°-135°
- temperatureAfter maintaining at 130°-140° for 30 mins
- temperaturethe viscous product was cooled to 100°
- extractionBasification and extraction with chloroform
- customgave crude amine
- customafter solvent evaporation
- distillationDistillation
출처 및 근거
- ORD 기록
- ord-b62e64ae25184cb0b39b044cb3a90ccc
- 출처 데이터셋
- uspto-grants-1984_04
- 특허 번호
- US04442286
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