Methylhydrazine → 3,5-Dibromo-4-[(2-methylhydrazinylidene)methyl]pyridine
反応式
[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]参加物
4
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-3440c0b7dbd44ac0bb3bfa89650d2587
- 出典データセット
- uspto-grants-2015_01
- 特許番号
- US08933224B2
反応ノート
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