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 67260280、化合物

HRID 2359027
ノート
印刷プレビュー

反応式

HRID 2359027 の反応式
[Cl:1][C:2]1[S:6][C:5]([C:7](=O)[CH2:8][C:9]2[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=2)=[CH:4][CH:3]=1.[CH:16]([NH:20][NH2:21])([CH2:18][CH3:19])[CH3:17].[CH2:22](N(CC)CC)C>ClCCl>[CH:16]([N:20]1[CH:22]=[C:8]([C:9]2[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=2)[C:7]([C:5]2[S:6][C:2]([Cl:1])=[CH:3][CH:4]=2)=[N:21]1)([CH2:18][CH3:19])[CH3:17].[CH:16]([N:20]1[C:7]([C:5]2[S:6][C:2]([Cl:1])=[CH:3][CH:4]=2)=[C:8]([C:9]2[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=2)[CH:22]=[N:21]1)([CH2:18][CH3:19])[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

6

反応物 3

HCID 8471TriethylamineHCID 547690sec-ButylhydrazineHCID 65583291HCID 65583291、化合物

生成物 2

HCID 67260280HCID 67260280、化合物収率 21%HCID 67260571HCID 67260571、化合物収率 16%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒

実験手順

A mixture of 1-(5-chloro-2-thienyl)-2-(pyridin-4-yl)ethanone (0.68 mmol), secbutylhydrazin (1.37 mmol) and triethylamine (1.37 mmol) in 5 mL dichloromethane was refluxed for 2.5 h. The solvent was evaporated under reduced pressure and the residue was partitioned between ethyl acetate and water. The aqueous layer was extracted with ethyl acetate and the combined organic extracts were dried over MgSO4 filtered and concentrated. The residue was purified by chromatography on silica gel (dichloromethane:methanol 100:1 to 20:1) to afford 37 mg of 4-[1-sec-butyl-3-(5-chloro-2-thienyl)-1H-pyrazol-4-yl]pyridine (16% yield) and 48 mg of 4-[1-sec-butyl-5-(5-chloro-2-thienyl)-1H-pyrazol-4-yl]pyridine (21% yield).

後処理

  1. temperaturewas refluxed for 2.5 h
  2. customThe solvent was evaporated under reduced pressure
  3. customthe residue was partitioned between ethyl acetate and water
  4. extractionThe aqueous layer was extracted with ethyl acetate
  5. dry with materialthe combined organic extracts were dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was purified by chromatography on silica gel (dichloromethane:methanol 100:1 to 20:1)

出典と根拠

ORDレコード
ord-836c52c166684ccfa282695d0e5143ee
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08685974B2

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