Methylhydrazine → 3,5-Dibromo-4-[(2-methylhydrazinylidene)methyl]pyridine
반응식
[CH3:1][NH:2][NH2:3].[Br:4][C:5]1[CH:6]=[N:7][CH:8]=[C:9]([Br:13])[C:10]=1[CH:11]=O>CC(O)C>[Br:4][C:5]1[CH:6]=[N:7][CH:8]=[C:9]([Br:13])[C:10]=1[CH:11]=[N:3][NH:2][CH3:1]참가 물질
4
실험 절차
Methylhydrazine (1.06 mL, 19.3 mmol) was added to a solution of 3,5-dibromopyridine-4-carbaldehyde (3.4 g, 13 mmol) in 2-propanol (20 mL). After 3 hours at room temperature, the reaction mixture was concentrated in vacuo, dissolved in ethyl acetate, and washed with saturated aqueous sodium chloride solution. The organic layer was dried over magnesium sulfate, filtered, and concentrated under reduced pressure to afford the product as a solid. Yield: 3.20 g, 10.9 mmol, 84%. 1H NMR (400 MHz, DMSO-d6) δ 8.62 (s, 2H), 7.24-7.26 (m, 1H), 2.89-2.91 (m, 3H).
후처리
- concentrationthe reaction mixture was concentrated in vacuo
- dissolutiondissolved in ethyl acetate
- washwashed with saturated aqueous sodium chloride solution
- dry with materialThe organic layer was dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-d2acf8ad5e054793abc2d5c0f161a01b
- 출처 데이터셋
- uspto-grants-2016_03
- 특허 번호
- US09296761B2
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