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HCID 66839446、化合物 → HCID 66839152、化合物

HRID 546746
ノート
印刷プレビュー

反応式

HRID 546746 の反応式
[CH3:1][O:2][C:3]1[N:8]=[C:7](/[CH:9]=[C:10](\[CH3:18])/[C:11]([O:13]C(C)(C)C)=[O:12])[CH:6]=[CH:5][C:4]=1[N:19]1[CH:23]=[C:22]([CH3:24])[N:21]=[CH:20]1>FC(F)(F)C(O)=O.C(Cl)Cl>[CH3:1][O:2][C:3]1[N:8]=[C:7](/[CH:9]=[C:10](\[CH3:18])/[C:11]([OH:13])=[O:12])[CH:6]=[CH:5][C:4]=1[N:19]1[CH:23]=[C:22]([CH3:24])[N:21]=[CH:20]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 66839446HCID 66839446、化合物

生成物 1

HCID 66839152HCID 66839152、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

A mixture of 6-chloro-2-methoxy-3-(4-methyl-1H-imidazol-1-yl)pyridine (400 mg), an allylpalladium chloride dimer (32.8 mg), tri-o-tolylphosphine (54.4 mg), sodium acetate (441 mg), dimethylacetamide (0.640 mL), tert-butyl methacrylate (0.724 mL) and toluene (2 mL) was stirred in a nitrogen atmosphere at 120° C. for 3.5 hours. The reaction solution was left to cool to room temperature. Then, a silica gel was added and the reaction solution was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system) to obtain 313 mg of tert-butyl (E)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]-2-methylacrylate. The ester was diluted with trifluoroacetic acid (2.48 mL) and methylene chloride (2.48 mL), and the reaction solution was stirred at room temperature for 3.5 hours. The reaction solution was concentrated under reduced pressure to obtain 260 mg of the title compound. The property value of the compound is as follows.

後処理

  1. concentrationThe reaction solution was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-2b7f47c86d27487cb447b1340531e7c3
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07935815B2

反応ノート

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