Acetonitrile → N-[4-(2-Formylhydrazinyl)phenyl]-3-nitrobenzene-1-sulfonamide
반응식
CN(C)C(=O)C.C(#N)C.C(N(CC)CC)C.[N+:17]([C:20]1[CH:21]=[C:22]([S:26](Cl)(=[O:28])=[O:27])[CH:23]=[CH:24][CH:25]=1)([O-:19])=[O:18].[NH2:30][C:31]1[CH:36]=[CH:35][C:34]([NH:37][NH:38][CH:39]=[O:40])=[CH:33][CH:32]=1>>[N+:17]([C:20]1[CH:21]=[C:22]([S:26]([NH:30][C:31]2[CH:32]=[CH:33][C:34]([NH:37][NH:38][CH:39]=[O:40])=[CH:35][CH:36]=2)(=[O:28])=[O:27])[CH:23]=[CH:24][CH:25]=1)([O-:19])=[O:18]참가 물질
반응 조건
- 온도
- -5 °C
실험 절차
1 1 of N,N-dimethylacetoamide, 880 g of acetonitrile, and 285 g of triethylamine were added to and dissolved in 426 g of 2-(4-aminophenyl)-1-formylhydrazine under an atmosphere of nitrogen. The solution was cooled to -5° C., and 625 g of meta-nitrobenzenesulfonyl chloride was gradually added to the solution. During the addition, the mixture was agitated under cooling so that the temperature did not exceed -5° C. The resultant mixture was cooled at a temperature below -5° C. for 1.5 hours, then the temperature thereof was raised to a room temperature. Extraction was performed with 12 l of ethyl acetate and 12 l of saturated salt water. The organic layer was separated and then concentrated to 6 l. 3 l of n-hexane was added to the concentrate, and the obtained mixture was agitated at a room temperature for 30 minutes. The produced crystals were filtered off and washed with 500 g of ethyl acetate.
후처리
- additionDuring the addition
- temperatureunder cooling so that the temperature
- customdid not exceed -5° C
- temperaturethe temperature thereof was raised to a room temperature
- extractionExtraction
- customThe organic layer was separated
- concentrationconcentrated to 6 l
- addition3 l of n-hexane was added to the concentrate
- stirringthe obtained mixture was agitated at a room temperature for 30 minutes
- filtrationThe produced crystals were filtered off
- washwashed with 500 g of ethyl acetate
출처 및 근거
- ORD 기록
- ord-0bf31fcb2abe4d74926242db5cb6b0fa
- 출처 데이터셋
- uspto-grants-1990_08
- 특허 번호
- US04952483
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