Phosphorus oxychloride → 4-Chloro-5-iodonicotinonitrile
反応式
O[C:2]1[C:7]([C:8]#[N:9])=[CH:6][N:5]=[CH:4][C:3]=1[I:10].O=P(Cl)(Cl)[Cl:13]>>[Cl:13][C:2]1[C:7]([C:8]#[N:9])=[CH:6][N:5]=[CH:4][C:3]=1[I:10]参加物
3
反応条件
- 温度
- 100 °C
実験手順
A mixture of 4-hydroxy-5-iodonicotinonitrile (57.5 g, 234 mmol) and POCl3 (200 mL) was heated at 100° C. for 2 hours, cooled to room temperature and evaporated to remove excess POCl3. The residue was cooled in an ice-water bath, adjusted to pH 8-9 with aqueous 10 N NaOH and extracted with ethyl acetate. The combined organics were washed with water and brine, dried over magnesium sulfate and concentrated. The resulting solid residue was washed with a minimum amount of methanol and methylene chloride to give 46.5 g (75%) of 4-chloro-5-iodonicotinonitrile as a tan solid. Melting range: 120-122° C.
後処理
- temperaturecooled to room temperature
- customevaporated
- customto remove excess POCl3
- temperatureThe residue was cooled in an ice-water bath
- extractionextracted with ethyl acetate
- washThe combined organics were washed with water and brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- washThe resulting solid residue was washed with a minimum amount of methanol and methylene chloride
出典と根拠
- ORDレコード
- ord-ad1e09b81c2d467d8431361fd21df552
- 出典データセット
- uspto-grants-2010_08
- 特許番号
- US07781591B2
反応ノート
読み込み中…