Hydrazine hydrate (1:1) → (2,6-Dichloropyridin-3-YL)methanamine
반응식
[Cl:1][C:2]1[C:7]([CH2:8][N:9]2C(=O)C3=CC=CC=C3C2=O)=[CH:6][CH:5]=[C:4]([Cl:20])[N:3]=1.NN.O>CCO.CN(C=O)C>[Cl:1][C:2]1[C:7]([CH2:8][NH2:9])=[CH:6][CH:5]=[C:4]([Cl:20])[N:3]=1참가 물질
5
실험 절차
In a mixture of 50 ml EtOH and 20 ml DMF was dissolved 3.1 g (0.01 mole) of N-(2,6-dichloro-3-pyridylmethyl)phthalimide under heating, followed by addition of 0.75 g (0.015 mole) of H2NNH2.H2O under reflux. After 1 hour of refluxing, EtOH and DMF were distilled off. To the residue were added 10 ml of concentrated hydrochloric acid and 5 ml of water, and the mixture was refluxed for 30 minutes. The resulting crystals were filtered off and the filtrate was neutralized with NaHCO3 and extracted with CH2Cl2 (30 ml×3). The extract was dried over MgSO4 and the solvent was distilled off to give 1.45 g of the title compound as a yellow oil.
후처리
- temperatureunder heating
- temperatureunder reflux
- temperatureAfter 1 hour of refluxing
- distillationEtOH and DMF were distilled off
- additionTo the residue were added 10 ml of concentrated hydrochloric acid and 5 ml of water
- temperaturethe mixture was refluxed for 30 minutes
- filtrationThe resulting crystals were filtered off
- extractionextracted with CH2Cl2 (30 ml×3)
- dry with materialThe extract was dried over MgSO4
- distillationthe solvent was distilled off
출처 및 근거
- ORD 기록
- ord-b13da614123340808572bea7820ba634
- 출처 데이터셋
- uspto-grants-1998_12
- 특허 번호
- US05849768
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