Isoamyl Nitrite → Benzothiazolone
反応式
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]参加物
4
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-f80d8b6e0dc34288bae22bdcf3a75cf6
- 出典データセット
- uspto-grants-1989_01
- 特許番号
- US04797399
反応ノート
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