ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Potassium Carbonate → 2-(2,4-Dichlorophenyl)-1-(1,2,4-triazol-1-yl)-3-(5-trifluoromethylimidazol-1-yl)-propan-2-ol

HRID 1583761
ノート
印刷プレビュー

反応式

HRID 1583761 の反応式
[F:1][C:2]([F:9])([F:8])[C:3]1[N:4]=[CH:5][NH:6][CH:7]=1.S(O)(=O)(=O)C.[Cl:15][C:16]1[CH:21]=[C:20]([Cl:22])[CH:19]=[CH:18][C:17]=1[C:23]1([CH2:26][N:27]2[CH:31]=[N:30][CH:29]=[N:28]2)[CH2:25][O:24]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[Cl:15][C:16]1[CH:21]=[C:20]([Cl:22])[CH:19]=[CH:18][C:17]=1[C:23]([OH:24])([CH2:25][N:4]1[C:3]([C:2]([F:9])([F:8])[F:1])=[CH:7][N:6]=[CH:5]1)[CH2:26][N:27]1[CH:31]=[N:30][CH:29]=[N:28]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 867396002-(2,4-Dichlorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane methanesulphonateHCID 178418921HCID 178418921、化合物

生成物 1

HCID 202583642-(2,4-Dichlorophenyl)-1-(1,2,4-triazol-1-yl)-3-(5-trifluoromethylimidazol-1-yl)-propan-2-ol収率 1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

実験手順

A mixture of 4-trifluoromethylimidazole (0.7 g, 5 mmole), 2-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-ylmethyl)-oxirane mesylate salt (1.88 g, 5 mmole) and anhydrous potassium carbonate (2.0 g, 14 mmole) in dry N,N-dimethylformamide (20 ml) was heated at 75°-80° C. for 18 hours. The solvent was evaporated under vacuum and the residue was partitioned between water (20 ml) and methylene chloride (50 ml). The aqueous layer was separated and extracted twice with methylene chloride (30 ml). The organic layers were combined, dried over magnesium sulphate and evaporated to yield the crude product containing the 4- and 5-trifluoromethyl-imidazolyl isomers. The residue was chromatographed on silica eluting with a mixture of hexane, isopropyl alcohol and concentrated ammonium hydroxide (80:20:1.5); fractions containing the minor component were evaporated and the product recrystallised from a mixture of acetone and water to give the desired title compound (0.02 g, 1%), m.p. 190°-192° C.

後処理

  1. temperaturewas heated at 75°-80° C. for 18 hours
  2. customThe solvent was evaporated under vacuum
  3. customthe residue was partitioned between water (20 ml) and methylene chloride (50 ml)
  4. customThe aqueous layer was separated
  5. extractionextracted twice with methylene chloride (30 ml)
  6. dry with materialdried over magnesium sulphate
  7. customevaporated
  8. customto yield the crude product
  9. customThe residue was chromatographed on silica eluting with a mixture of hexane, isopropyl alcohol and concentrated ammonium hydroxide (80:20:1.5)
  10. additionfractions containing the minor component
  11. customwere evaporated
  12. customthe product recrystallised from a mixture of acetone and water

出典と根拠

ORDレコード
ord-111e71b6ea584342a2b1fd4b45b44227
出典データセット
uspto-grants-1985_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04554286

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート