2,3-Dichloroaniline → 2-amino-4,5-dichlorobenzothiazole
反応式
[Cl:1][C:2]1[C:8]([Cl:9])=[CH:7][CH:6]=[CH:5][C:3]=1[NH2:4].[S-:10][C:11]#[N:12].[K+].BrBr>C(O)(=O)C>[NH2:12][C:11]1[S:10][C:5]2[CH:6]=[CH:7][C:8]([Cl:9])=[C:2]([Cl:1])[C:3]=2[N:4]=1参加物
5
実験手順
To a solution of 2,3-dichloroaniline (1.0 g; 6.17 mmol) in glacial acetic acid (30 ml) was added potassium thiocyanate (3.6 g; 37 mmol) and the mixture was stirred at ambient temperature until a clear solution had formed. Bromine (0.48 ml; 9.26 mmol) was added dropwise and the reaction mixture was stirred at ambient temperature for five hours. The solvent was removed under reduced pressure and the residue was diluted with water and rendered alkaline by addition of aqueous sodium hydroxide (6M). The product was filtered off, washed with water and dried to yield the desired product quantitatively.
後処理
- customhad formed
- stirringthe reaction mixture was stirred at ambient temperature for five hours
- customThe solvent was removed under reduced pressure
- additionthe residue was diluted with water
- additionby addition of aqueous sodium hydroxide (6M)
- filtrationThe product was filtered off
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-9760a974e5f24c6b88d727b803e4bba9
- 出典データセット
- uspto-grants-2004_07
- 特許番号
- US06759422B2
反応ノート
読み込み中…