Potassium Cyanide → HCID 84725891、化合物
反応式
[Br:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][N:5]=[C:4]([CH2:10]Br)[CH:3]=1.[C-:12]#[N:13].[K+]>CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-].O.C(Cl)Cl>[Br:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][N:5]=[C:4]([CH2:10][C:12]#[N:13])[CH:3]=1参加物
6
反応条件
- 温度
- 50 °C
実験手順
A suspension of 4-bromo-2-bromomethyl-5-methoxy-pyridine (Step AL2) (1.2 g, 4.3 mmol), KCN (417 mg, 6.4 mmol) and aliquat 336 (35 mg, 0.085 mmol) in H2O was stirred at 50° C. for 2 h. The reaction mixture was dissolved in CH2Cl2, extracted with a saturated aqueous solution of NaHCO3, washed with brine, dried (Na2SO4), filtered and concentrated. The crude product was purified by silica gel column chromatography (hexane/EtOAc, 100:0→1:1). tR: 3.83 min (HPLC 7).
後処理
- extractionextracted with a saturated aqueous solution of NaHCO3
- washwashed with brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
- customThe crude product was purified by silica gel column chromatography (hexane/EtOAc, 100:0→1:1)
出典と根拠
- ORDレコード
- ord-34a88bbcc41549bcacc92f45dc91fda3
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09365576B2
反応ノート
読み込み中…