반응식
C[O-:2].[Na+].[Na].NO.Cl.C[N:9](C)[CH:10]=[N:11][C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:13]=1[CH3:19]>CO.O>[Cl:18][C:15]1[CH:16]=[CH:17][C:12]([NH:11][CH:10]=[N:9][OH:2])=[C:13]([CH3:19])[CH:14]=1참가 물질
실험 절차
To a sodium methoxide solution prepared by dissolving 19 grams of sodium metal in 250 milliliters of methanol was added 56 grams of hydroxylamine:hydrochloride in 300 milliliters of methanol. To the resulting mixture was added 98 grams (0.5 mole) of N,N-dimethyl-N'-(4-chloro-2-methylphenyl)methanimidamide. The mixture was stirred at room temperature for 18 hours. The solid reaction product was recovered by filtration and the filtrate concentrated by evaporation under reduced pressure. The residue and the solid reaction product (filter cake) were suspended in water, collected by filtration, water washed and recrystallized from ethanol. The N-(4-chloro-2-methylphenyl)-N'-hydroxymethanimidamide product was recovered in a yield of 81.7 grams (89% of theoretical) and melted at 171°-171.5° C.
후처리
- customThe solid reaction product
- filtrationwas recovered by filtration
- concentrationthe filtrate concentrated by evaporation under reduced pressure
- customThe residue and the solid reaction product (filter cake)
- filtrationcollected by filtration, water
- washwashed
- customrecrystallized from ethanol
- customThe N-(4-chloro-2-methylphenyl)-N'-hydroxymethanimidamide product was recovered in a yield of 81.7 grams (89% of theoretical) and melted at 171°-171.5° C.
출처 및 근거
- ORD 기록
- ord-dbd04e5c2d42444180cea3c79f92479a
- 출처 데이터셋
- uspto-grants-1980_12
- 특허 번호
- US04237168
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