Morpholine → 4-(4-Morpholinobenzoyl)-nitrobenzene

HRID 2121023노트

반응식

HRID 2121023 반응식
F[C:2]1[CH:18]=[CH:17][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.[NH:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1.C(=O)([O-])[O-].[K+].[K+]>CS(C)=O.O>[O:22]1[CH2:23][CH2:24][N:19]([C:2]2[CH:18]=[CH:17][C:5]([C:6]([C:8]3[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=3)=[O:7])=[CH:4][CH:3]=2)[CH2:20][CH2:21]1

참가 물질

6

반응물 3

HCID 8083MorpholineHCID 11430Potassium CarbonateHCID 97658Methanone, (4-fluorophenyl)(4-nitrophenyl)-

생성물 1

HCID 218770174-(4-Morpholinobenzoyl)-nitrobenzene수율 91.3%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

반응 조건

온도
105 °C

실험 절차

A mixture containing 4-(4-fluorobenzoyl)-nitrobenzene (1.96 g, 8 mmol), morpholine (0.84 g, 9.6 mmol), and potassium carbonate (1.33 g, 9.6 mmol) in dimethyl sulfoxide (15 mL) was heated to 100-110° C. for 12 hours. The reaction mixture was cooled to room temperature and diluted with cold water, and filtered. The crude product was washed several times with water and dried to give 4-(4-morpholinobenzoyl)-nitrobenzene (2.28 g, 91%), m.p. 173-175° C., and was used in the next step without further purification.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationfiltered
  3. washThe crude product was washed several times with water
  4. customdried

출처 및 근거

ORD 기록
ord-ae2b32f7eba54f8da01ac958c65f8b44
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06693200B2

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