Water → N-methoxycarbonyl-3-(2-trans-butenyl)oxy-4-methoxyaniline

HRID 1090122ノート

反応式

HRID 1090122 の反応式
[CH3:1][O:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]([OH:14])[CH:7]=1)=[O:4].C(=O)([O-])[O-].[K+].[K+].[CH2:21](Cl)/[CH:22]=[CH:23]/[CH3:24].O>CN(C)C=O.C(OCC)(=O)C>[CH3:1][O:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]([O:14]/[CH:21]=[CH:22]/[CH2:23][CH3:24])[CH:7]=1)=[O:4]

参加物

7

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 637923(2E)-1-Chloro-2-buteneHCID 15675233HCID 15675233、化合物

生成物 1

HCID 86745378N-methoxycarbonyl-3-(2-trans-butenyl)oxy-4-methoxyaniline収率 91.2%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

The N-methoxycarbonyl-3-hydroxy-4-methoxyaniline (34.0 g) was dissolved in dimethylformamide (200 ml). Potassium carbonate (29.0 g) and trans-crotyl chloride (32.2 g) were added to the solution, and the mixture was stirred at room temperature for 5 hours. Water was added to the reaction mixture, and extraction was carried out with ethyl acetate. The extract was washed with saturated saline and dried over sodium sulfate, and the solvent was distilled off under reduced pressure. The crude crystal thus obtained was recrystallized from ethyl acetate-n-hexane to obtain N-methoxycarbonyl-3-(2-trans-butenyl)oxy-4-methoxyaniline (39.5 g).

後処理

  1. washThe extract was washed with saturated saline
  2. dry with materialdried over sodium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe crude crystal thus obtained
  5. customwas recrystallized from ethyl acetate-n-hexane

出典と根拠

ORDレコード
ord-0e0f9253ae06473b996fea191fd901bd
出典データセット
uspto-grants-1992_01
特許番号
US05081121

反応ノート

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