Isoamyl Nitrite → Benzothiazolone
반응식
N1(C(C[N:10]2[C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=3[S:12][C:11]2=[O:19])=O)CCNCC1.N(OCCC(C)C)=O>C(Cl)(Cl)Cl>[S:12]1[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[NH:10][C:11]1=[O:19]참가 물질
4
실험 절차
To a solution of 3-[(1-piperazinyl)carbonylmethyl]-2-benzothiazolinone (3.0 g) in chloroform (50 ml) was added dropwise isoamyl nitrite (7.3 ml), for a period of 10 minutes below 20° C. The mixture was stirred for 18 hours at ambient temperature. Then, the reaction mixture was extracted with chloroform. The extract was washed with water, dried over magnesium sulfate and evaporated to give a crystalline product, which was recrystallized from a mixture of ethyl acetate and ethanol to give 3-[4-nitroso-1-piperazinyl)carbonylmethyl]-2-benzothiazolinone (2.54 g) as needles.
후처리
- extractionThen, the reaction mixture was extracted with chloroform
- washThe extract was washed with water
- dry with materialdried over magnesium sulfate
- customevaporated
- customto give a crystalline product, which
- customwas recrystallized from a mixture of ethyl acetate and ethanol
출처 및 근거
- ORD 기록
- ord-f80d8b6e0dc34288bae22bdcf3a75cf6
- 출처 데이터셋
- uspto-grants-1989_01
- 특허 번호
- US04797399
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