반응식
[N:1]1[C:8]([Cl:9])=[N:7][C:5](Cl)=[N:4][C:2]=1[Cl:3].Cl.[NH2:11][CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14].C(=O)(O)[O-].[Na+]>>[Cl:9][C:8]1[N:1]=[C:2]([Cl:3])[N:4]=[C:5]([NH:11][CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])[N:7]=1참가 물질
4
실험 절차
36.9 g of cyanuric chloride, 27.9 g of ethyl glycinate hydrochloride and 33.6 g of sodium bicarbonate were heated under reflux in 200 ml of dioxanefor 30 minutes. At the end of this time, the dioxane was removed by distillation under reduced pressure, and a mixture of ethyl acetate and water was added to the resulting residue, after which the mixture was shaken. The ethyl acetate layer was separated, dried and concentrated by evaporation under reduced pressure, and the resulting residue was recrystallized from a mixture of hexane and ethyl acetate, to yield 45.0 gof the title compound as crystals melting at 82° to 87° C.
후처리
- temperatureunder reflux in 200 ml of dioxanefor 30 minutes
- customAt the end of this time, the dioxane was removed by distillation under reduced pressure
- additiona mixture of ethyl acetate and water
- additionwas added to the resulting residue
- customThe ethyl acetate layer was separated
- customdried
- concentrationconcentrated by evaporation under reduced pressure
- customthe resulting residue was recrystallized from a mixture of hexane and ethyl acetate
출처 및 근거
- ORD 기록
- ord-a263c55c9326424cab865273cb512687
- 출처 데이터셋
- uspto-grants-1995_08
- 특허 번호
- US05446144
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