Ethylenediamine → 7-Phenyl-1,2,3,4-tetrahydro-5H-1,4-diazepin-5-one
반응식
[CH2:1]([NH2:4])[CH2:2][NH2:3].[C:5]([CH2:13][C:14](OCC)=[O:15])(=O)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>N1C=CC=CC=1>[C:6]1([C:5]2[NH:4][CH2:1][CH2:2][NH:3][C:14](=[O:15])[CH:13]=2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1참가 물질
4
반응 조건
- 온도
- 180 °C
실험 절차
30 g ethylenediamine were added to 96 g ethyl benzoylacetate in 200 ml pyridine and the mixture was boiled under reflux for five hours. Then the pyridine was distilled off and the residue was heated to 180° C. for one hour. After cooling, 500 ml of dichloromethane were added, and the reaction mixture was heated to 40° C. until dissolution occurred. Precipitation with acetone yielded 21.7 g 7-phenyl-1,2,3,4-tetrahydro-1,4-diazepin-5-one having a melting point of 206-214° C.
후처리
- temperatureunder reflux for five hours
- distillationThen the pyridine was distilled off
- temperatureAfter cooling
- addition500 ml of dichloromethane were added
- temperaturethe reaction mixture was heated to 40° C. until dissolution
- customPrecipitation with acetone
출처 및 근거
- ORD 기록
- ord-6a0993a0d06a40dca41e53dee3823912
- 출처 데이터셋
- uspto-grants-2000_03
- 특허 번호
- US06040303
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