Ammonium thiocyanate → HCID 22400378、化合物
反応式
Cl.[Cl:2][C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH2:5][NH2:6].[S-:11][C:12]#[N:13].[NH4+]>O>[Cl:2][C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH2:5][NH:6][C:12]([NH2:13])=[S:11]参加物
4
実験手順
A solution of 2-chlorobenzylamine hydrochloride (41 g, 0.23 mol) and ammonium thiocyanate (19.28 g, 0.253 mol) in water (170 mL) was heated on the steam bath for 18 hours. This mixture was concentrated in vacuo, and the residue was taken up in toluene (1 L) and azeotroped with a Dean-Stark head. The residue was triturated with wet diethyl ether to provide 27.6 g (60%) of 1-(2-chlorophenyl)methyl thiourea. The product was recrystallized from ethanol; mp 120°-122° C.
後処理
- concentrationThis mixture was concentrated in vacuo
- customazeotroped with a Dean-Stark head
- customThe residue was triturated with wet diethyl ether
出典と根拠
- ORDレコード
- ord-3953e9b7c30c4e5e8fe42d37f310e41c
- 出典データセット
- uspto-grants-1996_06
- 特許番号
- US05530017
反応ノート
読み込み中…