反応式
[Cl:1][C:2]1[S:3][C:4]2[C:10]([N:11]=[C:12]=[S:13])=[C:9]([F:14])[CH:8]=[C:7]([Cl:15])[C:5]=2[N:6]=1.Cl.[NH2:17][C:18]1[NH:19][CH2:20][C:21]([CH3:24])([CH3:23])[CH:22]=1.[OH-].[Na+].BrBr>ClCCl.O>[Cl:1][C:2]1[S:3][C:4]2[C:10]([N:11]=[C:12]3[S:13][N:17]=[C:18]4[CH2:22][C:21]([CH3:24])([CH3:23])[CH2:20][N:19]34)=[C:9]([F:14])[CH:8]=[C:7]([Cl:15])[C:5]=2[N:6]=1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 2 °C
実験手順
A solution of 2 g 2,4-dichloro-6-fluoro-7-isothiocyanatobenzothiazole in 10 ml dichloromethane was added, dropwise, at 0° C., to a suspension of 1.1 g 2-amino-4,4-dimethylpyrroline hydrochloride in 20 ml dichloromethane. A solution of 0.3 g sodium hydroxide and 6 ml water was added, dropwise, at 2° C. to this mixture which was stirred for 3 hours, whereby the temperature rose to 20° C. The mixture was cooled to -10° C. and a solution of 1 g bromine in 10 ml dichloromethane was added, dropwise, slowly and the mixture stirred for I hour whereby the temperature rose to 10° C. The solution was washed with water and with dilute caustic soda, dried over magnesium sulfate and concentrated. The residue was recrystallised from diisopropyl ether. Yield: 1.5 g=53% of theory m.p.: 134°-136° C.
後処理
- customrose to 20° C
- temperatureThe mixture was cooled to -10° C.
- stirringdropwise, slowly and the mixture stirred for I hour whereby the temperature
- customrose to 10° C
- washThe solution was washed with water and with dilute caustic soda
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- customThe residue was recrystallised from diisopropyl ether
出典と根拠
- ORDレコード
- ord-d804bd441201440e948ae6abc9e51e2d
- 出典データセット
- uspto-grants-1995_06
- 特許番号
- US05424443
関連ノート
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