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

Triethylamine → HCID 59346927、化合物

HRID 20549
ノート
印刷プレビュー

反応式

HRID 20549 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:20]=[C:21]([O:23][C@@H:24]([CH3:28])[CH2:25][O:26][CH3:27])[CH:22]=1)[C:5]([NH:7][C:8]1[CH:12]=[CH:11][N:10]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[N:9]=1)=[O:6].C(N([CH2:34][CH3:35])CC)C>C(Cl)Cl.C([O-])(=O)C.[Cu+2].C([O-])(=O)C>[CH2:16]([O:15][C:13]([C:35]1[CH:34]=[CH:21][C:22]([O:1][C:2]2[CH:3]=[C:4]([CH:20]=[C:21]([O:23][C@@H:24]([CH3:28])[CH2:25][O:26][CH3:27])[CH:22]=2)[C:5]([NH:7][C:8]2[CH:12]=[CH:11][N:10]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[N:9]=2)=[O:6])=[CH:2][CH:3]=1)=[O:14])[CH3:17]
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 2

HCID 8471TriethylamineHCID 59127185tert-Butyl 3-({3-hydroxy-5-[(1S)-2-methoxy-1-methylethoxy]benzoyl}amino)-1H-pyrazole-1-carboxylate

生成物 1

HCID 59346927HCID 59346927、化合物収率 39%

試薬・触媒・溶媒 2

HCID 8895Cupric acetate触媒HCID 6344Dichloromethane溶媒

実験手順

tert-Butyl 3-({3-hydroxy-5-[(1S)-2-methoxy-1-methylethoxy]benzoyl}amino)-1H-pyrazole-1-carboxylate (391 mg, 1 mmol), ethyl-4-boronic acid benzoate (388 mg, 2.0 equiv), copper (II) acetate (363 mg, 2.0 equiv) and triethylamine (0.7 mL; 5.0 equiv) were suspended in dry DCM over freshly activated powdered 4A molecular sieves (ca. 1 g) for 7 hours under an ambient atmosphere. Reaction mixture filtered through diatomaceous earth was washed with DCM (×3). Filtrate concentrated in vacuo, taken up in ethyl acetate and washed with 1M hydrochloric acid, saturated sodium hydrogen carbonate, saturated brine and dried (MgSO4). Filtered, filtrate concentrated in vacuo and chromatographed (0-50% ethyl acetate/isohexane) to give a brown oil (210 mg, 39%).

後処理

  1. customfor 7 hours
  2. customReaction mixture
  3. filtrationfiltered through diatomaceous earth
  4. washwas washed with DCM (×3)
  5. concentrationFiltrate concentrated in vacuo
  6. washwashed with 1M hydrochloric acid, saturated sodium hydrogen carbonate, saturated brine
  7. dry with materialdried (MgSO4)
  8. filtrationFiltered
  9. concentrationfiltrate concentrated in vacuo
  10. customchromatographed (0-50% ethyl acetate/isohexane)

出典と根拠

ORDレコード
ord-4c466e908bf046fc954dac86ac97a6e8
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07745475B2

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