Methanol → 6-(2-Oxoethyl)nicotinonitrile
反応式
[CH2:1]([C:4]1[N:9]=[CH:8][C:7]([C:10]#[N:11])=[CH:6][CH:5]=1)[CH:2]=C.C[OH:13]>C(Cl)Cl>[O:13]=[CH:2][CH2:1][C:4]1[N:9]=[CH:8][C:7]([C:10]#[N:11])=[CH:6][CH:5]=1参加物
4
反応条件
- 温度
- -70 °C
実験手順
A mixture of 6-(Prop-2-en-1-yl)pyridine-3-carbonitrile (4.8 g, 33 mmol) in 80 mL of DCM and 20 mL of MeOH was cooled to −70° C. Ozone was bubbled through the mixture until the mixture turned blue (about 20 minutes). The excess of ozone was removed by flush with N2 flow until the mixture turned colorless. 5 mL of Me2S was added to the mixture which was then warmed slowly to room temperature and stirred for 2 hours. The solvent was removed under vacuum below 30° C. to afford the title compound which was used without further purification.
後処理
- customOzone was bubbled through the mixture until the mixture
- custom(about 20 minutes)
- customThe excess of ozone was removed
- customby flush with N2 flow until the mixture
- addition5 mL of Me2S was added to the mixture which
- temperaturewas then warmed slowly to room temperature
- customThe solvent was removed under vacuum below 30° C.
出典と根拠
- ORDレコード
- ord-9a02be7ad62f409aa48c5221d2671734
- 出典データセット
- uspto-grants-2015_04
- 特許番号
- US08999990B2
反応ノート
読み込み中…