Morpholine → 4-(4-Morpholinobenzoyl)-nitrobenzene

HRID 993374ノート

反応式

HRID 993374 の反応式
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

参加物

6

反応物 3

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

生成物 1

HCID 218770174-(4-Morpholinobenzoyl)-nitrobenzene収率 91.3%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

反応条件

温度
105 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-19d3f4ec38c443f889a6fc4522cede40
出典データセット
uspto-grants-2002_10
特許番号
US06472536B1

反応ノート

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