反応式
N[C:2]1[S:3][C:4]2[CH:10]=[C:9]([CH3:11])[CH:8]=[C:7]([Br:12])[C:5]=2[N:6]=1.[Br:13](O)(=O)=O.BrBr.N([O-])=O.[Na+].[OH-].[Na+]>>[Br:13][C:2]1[S:3][C:4]2[CH:10]=[C:9]([CH3:11])[CH:8]=[C:7]([Br:12])[C:5]=2[N:6]=1参加物
6
実験手順
4.7 g of 2-amino-4-bromo-6-methylbenzothiazole, 14 ml of 48% bromic acid solution and 10 g of bromine were introduced into a reaction vessel while keeping the temperature at 10° C. To this mixture was slowly added dropwise 10 ml of aqueous solution containing 3.5 g of sodium nitrite at 0° C. and the whole mixture was stirred for 2 hours. Then, 15 ml of 40% sodium hydroxide solution was slowly added dropwise while keeping the temperature below 20° C. and the reaction mixture was stirred for one hour and extracted with diethyl ether. The extract was dried with anhydrous sodium sulfate and evaporated to obtain the title compound in the form of transparent liquid (Yield: 91%).
後処理
- customat 10° C
- customthe temperature below 20° C.
- stirringthe reaction mixture was stirred for one hour
- extractionextracted with diethyl ether
- dry with materialThe extract was dried with anhydrous sodium sulfate
- customevaporated
出典と根拠
- ORDレコード
- ord-e2bb665e554a4ed2bafa8435ae6d0eff
- 出典データセット
- uspto-grants-1995_01
- 特許番号
- US05380735
関連ノート
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