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3-Aminophenol → HCID 54524025, 화합물

HRID 1417995
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인쇄 미리보기

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HRID 1417995 반응식
Cl[C:2]1[CH:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[CH:10]=2)[N:5]=[CH:4][N:3]=1.[NH2:16][C:17]1[CH:18]=[C:19]([OH:23])[CH:20]=[CH:21][CH:22]=1>C(Cl)Cl>[OH:23][C:19]1[CH:18]=[C:17]([CH:22]=[CH:21][CH:20]=1)[NH:16][C:2]1[CH:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[CH:10]=2)[N:5]=[CH:4][N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 115683-AminophenolHCID 51046229HCID 51046229, 화합물

생성물 1

HCID 54524025HCID 54524025, 화합물수율 39%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
140 °C

실험 절차

A mixture of 4-chloro-6-(3'-methylanilino)pyrimidine (9.56 g) and 3-aminophenol (5.22 g) was stirred and heated at 140° C. for 3 hours. The product so obtained was dissolved in methylene chloride and a few drops of methanol, and chromatographed on silica using a mixture of methylene chloride and methanol, increasing in polarity from pure methylene chloride to a 19:1 mixture of methylene chloride and methanol as eluent. The product so obtained was recrystallised from a mixture of ethyl acetate and hexane to give 4-(3'-hydroxyanilino)-6-(3'-methylanilino)pyrimidine in 39% yield, m.p. 188°-189° C.;

후처리

  1. customThe product so obtained
  2. customa few drops of methanol, and chromatographed on silica using
  3. additiona mixture of methylene chloride and methanol
  4. temperatureincreasing in polarity from pure methylene chloride to a 19:1 mixture of methylene chloride and methanol as eluent
  5. customThe product so obtained
  6. customwas recrystallised from a mixture of ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-71922d1d37464fe1a931186e3c008768
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05880130

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