Methanol → 4-Cyclopropylpyridin-3-amine
反応式
[Cl-].[NH4+].[CH:3]1([C:6]2[CH:11]=[CH:10][N:9]=[CH:8][C:7]=2[N+:12]([O-])=O)[CH2:5][CH2:4]1.CO>C1COCC1.C(Cl)(Cl)Cl.[Zn]>[CH:3]1([C:6]2[CH:11]=[CH:10][N:9]=[CH:8][C:7]=2[NH2:12])[CH2:5][CH2:4]1参加物
7
実験手順
Zinc powder (223.2 mg, 3.41 mmol) and ammonium chloride solution (365 mg, 6.8 mmol) were added to a stirred solution of 4-cyclopropyl-3-nitropyridine (I-1a: 70 mg, 0.426 mmol) in dry THF (2 mL) at 0° C. and the resulting mixture was stirred at room temperature for 1 hour. The reaction was monitored by TLC (10% methanol in CHCl3). The reaction mixture was filtered over celite bed and washed with THF and filtrate was concentrated. The residue was dissolved in ethyl acetate and washed with water and saturated brine and dried over sodium sulphate and concentrated to afford 450 mg of the product (100% yield).
後処理
- filtrationThe reaction mixture was filtered over celite bed
- washwashed with THF and filtrate
- concentrationwas concentrated
- dissolutionThe residue was dissolved in ethyl acetate
- washwashed with water and saturated brine
- dry with materialdried over sodium sulphate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-92509081ede143e1824eae99d56c09fe
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09339501B2
反応ノート
読み込み中…