Ethylenediamine → 6-Amino-4,5-dimethyl-3-pyridinecarbonitrile
반응식
Br[C:2]1[C:3]([CH3:10])=[C:4]([CH3:9])[C:5]([NH2:8])=[N:6][CH:7]=1.[C:11]([Cu])#[N:12].C(N)CN>CC(N(C)C)=O>[NH2:8][C:5]1[C:4]([CH3:9])=[C:3]([CH3:10])[C:2]([C:11]#[N:12])=[CH:7][N:6]=1참가 물질
5
반응 조건
- 온도
- 170 °C
실험 절차
A mixture of 5-bromo-3,4-dimethyl-pyridin-2-ylamine (500 mg, 2.49 mmol), CuCN (445 mg, 4.97 mmol) and DMA (3.5 mL) was stirred under nitrogen for 20 h at 170° C. The reaction mixture was cooled and added to 50 mL of a 20% aqueous solution of ethane-1,2-diamine. The layers were separated and the aqueous layer was extracted 3× with EtOAc. The combined organics were washed with water, followed by brine and dried over MgSO4. Concentration in vacuo afforded compound 850A (362 mg, 99%) as a white solid.
후처리
- temperatureThe reaction mixture was cooled
- customThe layers were separated
- extractionthe aqueous layer was extracted 3× with EtOAc
- washThe combined organics were washed with water
- dry with materialdried over MgSO4
- concentrationConcentration in vacuo
출처 및 근거
- ORD 기록
- ord-3a8a1cc6ca46400287f7ae17c122f53e
- 출처 데이터셋
- uspto-grants-2010_02
- 특허 번호
- US07655689B2
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