Morpholine → 1-(4-Chlorophenyl)-2-methyl-2-(morpholin-4-yl)propan-1-one
반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([O:13]C)[C:10]([CH3:12])([CH3:11])O2)=[CH:4][CH:3]=1.[NH:15]1[CH2:20][CH2:19][O:18][CH2:17][CH2:16]1>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8](=[O:13])[C:10]([CH3:11])([N:15]2[CH2:20][CH2:19][O:18][CH2:17][CH2:16]2)[CH3:12])=[CH:6][CH:7]=1참가 물질
3
실험 절차
85.1 g (0.4 mol) of 2-(4-chlorophenyl)-3,3-dimethyl-2-methoxyoxirane and 139.4 g (1.6 mols) of morpholine are combined and warmed to reflux temperature. After 22 hours the mixture is cooled and morpholine is removed by distillation. The residue is taken up in ether, and the solution is extracted with dilute hydrochloric acid. The hydrochloric acid solution is rendered alkaline and extracted with ether. The ether solution is dried with Na2SO4 and concentrated. The residue is recrystallised from ethanol.
후처리
- temperaturewarmed
- temperatureto reflux temperature
- temperatureAfter 22 hours the mixture is cooled
- custommorpholine is removed by distillation
- extractionthe solution is extracted with dilute hydrochloric acid
- extractionextracted with ether
- dry with materialThe ether solution is dried with Na2SO4
- concentrationconcentrated
- customThe residue is recrystallised from ethanol
출처 및 근거
- ORD 기록
- ord-d7deaa3223c6449ea636abe9f7f0b94e
- 출처 데이터셋
- uspto-grants-1986_04
- 특허 번호
- US04582862
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