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

tert-Butyl methacrylate → HCID 66839446、化合物

HRID 546745
ノート
印刷プレビュー

反応式

HRID 546745 の反応式
Cl[C:2]1[N:7]=[C:6]([O:8][CH3:9])[C:5]([N:10]2[CH:14]=[C:13]([CH3:15])[N:12]=[CH:11]2)=[CH:4][CH:3]=1.C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.C([O-])(=O)C.[Na+].[C:43]([O:48][C:49]([CH3:52])([CH3:51])[CH3:50])(=[O:47])[C:44]([CH3:46])=[CH2:45]>[CH2-]C=C.[CH2-]C=C.Cl[Pd+].Cl[Pd+].C1(C)C=CC=CC=1.CC(N(C)C)=O>[CH3:9][O:8][C:6]1[N:7]=[C:2](/[CH:45]=[C:44](\[CH3:46])/[C:43]([O:48][C:49]([CH3:52])([CH3:51])[CH3:50])=[O:47])[CH:3]=[CH:4][C:5]=1[N:10]1[CH:14]=[C:13]([CH3:15])[N:12]=[CH:11]1
参加物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 11448tert-Butyl methacrylateHCID 80271Tri-o-tolylphosphineHCID 517045Sodium AcetateHCID 86628513HCID 86628513、化合物

生成物 1

HCID 66839446HCID 66839446、化合物

試薬・触媒・溶媒 3

HCID 61538Palladium, di-mu-chlorobis(eta3-2-propenyl)di-触媒
HCID 1140Toluene溶媒
HCID 31374Dimethylacetamide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. waitThe reaction solution was left
  2. additionThen, a silica gel was added
  3. concentrationthe reaction solution was concentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system)

出典と根拠

ORDレコード
ord-1a6ccff7f5344086a8c634df1131230c
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

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