Hydrochloric Acid → HCID 18543276、化合物
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([S:9][CH2:10][C:11]#[N:12])[CH:5]=[C:6]([Cl:8])[CH:7]=1.O.Cl.[OH-].[Na+]>COCCOC>[Cl:8][C:6]1[CH:5]=[C:4]([S:9][CH2:10][CH2:11][NH2:12])[CH:3]=[C:2]([Cl:1])[CH:7]=1参加物
6
実験手順
To a solution of (3,5-dichlorophenylthio)acetonitrile (1.2 g) in 3.0 mL of ethylene glycol dimethyl ether is added 0.61 mL of 10 M borane dimethyl sulfide complex and the mixture heated at reflux for 0.5 hours. The reaction is cooled in an ice bath and 2.0 mL of water and 2.0 mL of concentrated hydrochloric acid is added. This mixture is heated at reflux for 0.5 hr. The clear solution is then cooled and basified with 5 N sodium hydroxide and extracted with ether. The ether extract is dried over potassium carbonate, filtered and concentrated to give 1.0 g of a colorless oil.
後処理
- temperaturethe mixture heated
- temperatureat reflux for 0.5 hours
- temperatureThe reaction is cooled in an ice bath
- temperatureThis mixture is heated
- temperatureat reflux for 0.5 hr
- temperatureThe clear solution is then cooled
- extractionextracted with ether
- extractionThe ether extract
- dry with materialis dried over potassium carbonate
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-c9033164acfd4afe857d5893b0b1b95c
- 出典データセット
- uspto-grants-2000_12
- 特許番号
- US06166028
反応ノート
読み込み中…