4-Aminophenol → HCID 18452583、化合物

HRID 1271037ノート

反応式

HRID 1271037 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 18452583HCID 18452583、化合物収率 24.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c27e4aaad69e476e981dc0c27e7b57f2
出典データセット
uspto-grants-2007_04
特許番号
US07205297B2

反応ノート

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