반응식
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]=1참가 물질
6
실험 절차
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%).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-e2bb665e554a4ed2bafa8435ae6d0eff
- 출처 데이터셋
- uspto-grants-1995_01
- 특허 번호
- US05380735
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