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

HRID 1090122노트

반응식

HRID 1090122 반응식
[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]

참가 물질

7

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 637923(2E)-1-Chloro-2-buteneHCID 15675233HCID 15675233, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-0e0f9253ae06473b996fea191fd901bd
출처 데이터셋
uspto-grants-1992_01
특허 번호
US05081121

반응 노트

불러오는 중…