4-Aminophenol → HCID 18452583, 화합물

HRID 1271037노트

반응식

HRID 1271037 반응식
[Cl:1][C:2]1[C:7]([C:8]#[C:9][C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=2)=[CH:6][N:5]=[CH:4][N:3]=1.[OH:17][C:18]1[CH:24]=[CH:23][C:21]([NH2:22])=[CH:20][CH:19]=1>C(O)C>[ClH:1].[Cl:16][C:13]1[CH:14]=[CH:15][C:10]([C:9]#[C:8][C:7]2[C:2]([NH:22][C:21]3[CH:23]=[CH:24][C:18]([OH:17])=[CH:19][CH:20]=3)=[N:3][CH:4]=[N:5][CH:6]=2)=[CH:11][CH:12]=1

참가 물질

4

반응물 2

HCID 4034-AminophenolHCID 184525694-Chloro-5-[(4-chlorophenyl)ethynyl]pyrimidine

생성물 1

HCID 18452583HCID 18452583, 화합물수율 24.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 0.28 g of 4-chloro-5-(4-Chlorophenylethynyl)pyrimidine, 10 mL of ethanol and 0.14 g of 4-hydroxyaniline was stirred at room temperature for 18 hours. The black mixture was evaporated in vacuo and the residue was triturated with dichloromethane, ethylacetate and acetonitrile. The combined organic extracts were absorbed on silica gel and evaporated in vacuo. The powder was added to a column of silica gel equilibrated in dichloromethane and eluted with the same solvent. The column was eluted with ethyl acetate and then 10% methanol in dichloromethane. These eluates on evaporation produced 100 mg of the 5-(4-chlorophenylethynyl)-4-(4-hydroxyanilino)pyrimidine hydrochloride as a muddy yellow powder.

후처리

  1. customThe black mixture was evaporated in vacuo
  2. customthe residue was triturated with dichloromethane, ethylacetate and acetonitrile
  3. customThe combined organic extracts were absorbed on silica gel
  4. customevaporated in vacuo
  5. additionThe powder was added to a column of silica gel
  6. washeluted with the same solvent
  7. washThe column was eluted with ethyl acetate
  8. customThese eluates on evaporation

출처 및 근거

ORD 기록
ord-c27e4aaad69e476e981dc0c27e7b57f2
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07205297B2

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