반응식
[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[C:7](=[O:11])[CH2:8][C:9]#[N:10].C(N(CC)CC)C.[N+:19]([C:22]1[CH:27]=[CH:26][C:25]([N:28]=[C:29]=[O:30])=[CH:24][CH:23]=1)([O-:21])=[O:20]>C1(C)C=CC=CC=1.CS(C)=O>[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[C:7](=[O:11])[CH:8]([C:29](=[O:30])[NH:28][C:25]1[CH:24]=[CH:23][C:22]([N+:19]([O-:21])=[O:20])=[CH:27][CH:26]=1)[C:9]#[N:10]참가 물질
실험 절차
The solution of 4.9 g of the 1-methyl-β-oxo-2-pyrrolpropionitrile in 50 ml of toluene, 5 ml of dimethylsulfoxide and 4 g of triethylamine is treated with the solution of 5.7 g of p-nitrophenylisocyanate in the minimum amount of toluene while stirring. After standing overnight it is evaporated and the residue taken up in methanol. The solution is filtered, diluted with water and 6 ml of triethylamine, washed with ethyl acetate, and the washings extracted once with 5% aqueous sodium hydroxide. The combined aqueous solutions are acidified with 5 N hydrochloric acid and the precipitate collected. It is washed with water, triturated with methanol-ethanol and recrystallized from dimethylformamide, to yield the 1-methyl-β-oxo-α-(p-nitrophenylcarbamoyl)-2-pyrrolpropionitrile melting at 245°-250° with decomposition.
후처리
- customit is evaporated
- filtrationThe solution is filtered
- additiondiluted with water and 6 ml of triethylamine
- washwashed with ethyl acetate
- extractionthe washings extracted once with 5% aqueous sodium hydroxide
- customthe precipitate collected
- washIt is washed with water
- customtriturated with methanol-ethanol
- customrecrystallized from dimethylformamide
출처 및 근거
- ORD 기록
- ord-4724d9ac5eb64a77a9945cca3c2ce5fa
- 출처 데이터셋
- uspto-grants-1981_03
- 특허 번호
- US04256759
연결된 노트
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