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

4-Chlorobenzaldehyde → 4-[5-(4-tert-Butyl-phenyl)-2-(4-chloro-phenyl)-3H-imidazol-4-yl]-pyridine

HRID 1418053
ノート
印刷プレビュー

反応式

HRID 1418053 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11]([CH:13]([C:22]2[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=2)O[Si](C(C)(C)C)(C)C)=O)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].C([O-])(=O)C.[NH4+:32].[Cl:33][C:34]1[CH:41]=[CH:40][C:37]([CH:38]=O)=[CH:36][CH:35]=1.[OH-].[NH4+:43]>C(O)(=O)C.C([O-])(=O)C.[Cu+2].C([O-])(=O)C.C(OCC)(=O)C>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([C:11]2[N:32]=[C:38]([C:37]3[CH:40]=[CH:41][C:34]([Cl:33])=[CH:35][CH:36]=3)[NH:43][C:13]=2[C:22]2[CH:23]=[CH:24][N:25]=[CH:26][CH:27]=2)=[CH:9][CH:10]=1)([CH3:2])([CH3:3])[CH3:4]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 77264-ChlorobenzaldehydeHCID 14923Ammonium HydroxideHCID 517165Ammonium AcetateHCID 674868814-Pyridyl-t-butydimethylsilyloxymethyl 4-t-butylphenyl ketone

生成物 1

HCID 98432394-[5-(4-tert-Butyl-phenyl)-2-(4-chloro-phenyl)-3H-imidazol-4-yl]-pyridine収率 59%

試薬・触媒・溶媒 3

HCID 8895
Cupric acetate
触媒
HCID 176Acetic Acid溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

A solution of 4-pyridyl-t-butydimethylsilyloxymethyl 4-t-butylphenyl ketone from Step C (170 mg, 0.44 mmol), copper (II) acetate (161 mg, 0.89 mmol), ammonium acetate (342 mg, 4.44 mmol) and 4-chlorobenzaldehyde (78 mg, 0.56 mmol) in acetic acid (3 mL) was heated to 110° C. for 5 h. The reaction mixture was then cooled to 0° C. and ice (4 g), ethyl acetate (4 mL) and concentrated ammonium hydroxide solution (4 mL) were added. After stirring for 30 min, the phases were separated and the aqueous layer extracted with ethyl acetate (2 times). The combined organic phases were successively washed with water (2 times) and saturated salt solution and dried over anhydrous sodium sulfate. The mixture was filtered and the solvent removed by rotoevaporation. The residue was purified by flash column chromatography on silica gel eluted with 0-3% methanol in methylene chloride to yield the title compound as a pale yellow solid 102 mg, 59% yield), mass spectrum (CI) m/e=388 (M+1)+.

後処理

  1. customthe phases were separated
  2. extractionthe aqueous layer extracted with ethyl acetate (2 times)
  3. washThe combined organic phases were successively washed with water (2 times) and saturated salt solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationThe mixture was filtered
  6. customthe solvent removed by rotoevaporation
  7. customThe residue was purified by flash column chromatography on silica gel
  8. washeluted with 0-3% methanol in methylene chloride

出典と根拠

ORDレコード
ord-8d4e00615b9a4d69934dcbf35ea0d131
出典データセット
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05880139

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート