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Acetic Acid → Methyl 3-(6-(4-phenoxyphenylamino)pyrimidin-4-ylamino)benzoate

HRID 577336
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인쇄 미리보기

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HRID 577336 반응식
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH:8][C:9]2[CH:10]=[C:11]([CH:16]=[CH:17][CH:18]=2)[C:12]([O:14][CH3:15])=[O:13])[CH:3]=1.[O:19]([C:26]1[CH:32]=[CH:31][C:29]([NH2:30])=[CH:28][CH:27]=1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.C(O)(=O)C>C(O)C>[O:19]([C:26]1[CH:27]=[CH:28][C:29]([NH:30][C:2]2[N:7]=[CH:6][N:5]=[C:4]([NH:8][C:9]3[CH:10]=[C:11]([CH:16]=[CH:17][CH:18]=3)[C:12]([O:14][CH3:15])=[O:13])[CH:3]=2)=[CH:31][CH:32]=1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 8764(4-Aminophenoxy)benzeneHCID 57708270Methyl 3-(6-chloropyrimidin-4-ylamino)benzoate

생성물 1

HCID 57708324Methyl 3-(6-(4-phenoxyphenylamino)pyrimidin-4-ylamino)benzoate수율 66%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
100 °C

실험 절차

To a stirring solution of methyl 3-(6-chloropyrimidin-4-ylamino)benzoate (1.0 g, 3.8 mmol) and 4-phenoxy aniline (0.703 g, 3.8 mmol) in ethanol (5 mL) was added acetic acid (0.22 mL) and the reaction mixture was heated at 100° C. for 48 h. The reaction mixture was cooled, ethanol was removed under reduced pressure and the residue was dissolved in ethyl acetate (50 mL). It was washed with NaHCO3 solution (5 mL) and brine (5 mL), was dried over Na2SO4 and was concentrated under reduced pressure. The residue was purified by column chromatography (SiO2, 60-120, chloroform/methanol, 9/1) to yield methyl 3-(6-(4-phenoxyphenylamino)pyrimidin-4-ylamino)benzoate (1 g, 66%) as an off-white solid.

후처리

  1. temperatureThe reaction mixture was cooled
  2. customethanol was removed under reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate (50 mL)
  4. washIt was washed with NaHCO3 solution (5 mL) and brine (5 mL)
  5. dry with materialwas dried over Na2SO4
  6. concentrationwas concentrated under reduced pressure
  7. customThe residue was purified by column chromatography (SiO2, 60-120, chloroform/methanol, 9/1)

출처 및 근거

ORD 기록
ord-c690ea4c957f4fe6af1e6bb837f1cb89
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09040541B2

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