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Water → HCID 135736655, 화합물

HRID 358809
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HRID 358809 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:10]2[N:15]=[CH:14][C:13]([C:16]3[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])=[CH:18][CH:17]=3)=[CH:12][N:11]=2)[CH:5]=[CH:6][C:7]=1[O:8]C.O>C(O)(=O)C.Br>[F:1][C:2]1[CH:3]=[C:4]([C:10]2[N:11]=[CH:12][C:13]([C:16]3[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])=[CH:18][CH:17]=3)=[CH:14][N:15]=2)[CH:5]=[CH:6][C:7]=1[OH:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 962WaterHCID 14745779HCID 14745779, 화합물

생성물 1

HCID 135736655HCID 135736655, 화합물수율 87.2%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 260Hydrogen Bromide용매

실험 절차

2.5 g of the 2-(3-fluoro-4-methoxyphenyl)-5-(4-heptylphenyl)pyrimidine obtained in Example 1 was dissolved in a mixture of 200 ml of acetic acid and 100 ml of 47% hydrobromic acid. The obtained solution was heated under reflux for 18 hours. The reaction mixture was allowed to cool to room temperature and 500 ml of water was added thereto. The crystals thus precipitated were filtered. The product thus obtained was purified by column chromatography (developing solvent: hexane: ethyl acetate 5:1) to thereby give 2.1 g of 2-(3-fluoro-4-hydroxyphenyl)-5-(4-heptylphenyl)pyrimidine. Yield: 87%.

후처리

  1. temperatureThe obtained solution was heated
  2. temperatureunder reflux for 18 hours
  3. customThe crystals thus precipitated
  4. filtrationwere filtered
  5. customThe product thus obtained
  6. customwas purified by column chromatography (developing solvent: hexane: ethyl acetate 5:1)

출처 및 근거

ORD 기록
ord-4042a832bff84b12917b349155f481f5
출처 데이터셋
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04997942

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