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Dichloromethane → 4-(3-(1,3-Dioxolan-2-yl)-4-nitrophenyl)morpholine

HRID 1487192
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반응식

HRID 1487192 반응식
Cl[C:2]1[CH:3]=[CH:4][C:5]([N+:13]([O-:15])=[O:14])=[C:6]([CH:8]2[O:12][CH2:11][CH2:10][O:9]2)[CH:7]=1.ClCCl.[NH:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1>>[O:9]1[CH2:10][CH2:11][O:12][CH:8]1[C:6]1[CH:7]=[C:2]([N:19]2[CH2:24][CH2:23][O:22][CH2:21][CH2:20]2)[CH:3]=[CH:4][C:5]=1[N+:13]([O-:15])=[O:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6344DichloromethaneHCID 8083MorpholineHCID 2673852-(5-Chloro-2-nitrophenyl)-1,3-dioxolane

생성물 1

HCID 866996844-(3-(1,3-Dioxolan-2-yl)-4-nitrophenyl)morpholine수율 97.1%

실험 절차

2-(5-Chloro-2-nitrophenyl)-1,3-dioxolane (13.4 g, 58.4 mmol) was dissolved in morpholine (150 mL). The mixture was then heated to reflux for 16 hours. Cooling to room temperature, dichloromethane was added. The organic phase was washed with water, dried over anhydrous sodium sulfate, evaporated and purified by silica gel chromatography to afford the product 4-(3-(1,3-dioxolan-2-yl)-4-nitrophenyl)morpholine (15.9 g, yield 97.1%).

후처리

  • temperatureThe mixture was then heated
  • temperatureto reflux for 16 hours
  • washThe organic phase was washed with water
  • dry with materialdried over anhydrous sodium sulfate
  • customevaporated
  • custompurified by silica gel chromatography
  • 출처 및 근거

    ORD 기록
    ord-4a084a21f93a422d9e51761a639bc4a8
    출처 데이터셋
    uspto-grants-2016_08
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US09428508B2

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