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

Water → N-[2-(3,5-dichloropyridin-2-yl)-2-(propoxyimino)ethyl]-2-(trifluoromethyl)benzamide

HRID 55988
ノート
印刷プレビュー

反応式

HRID 55988 の反応式
[CH2:1]([O:4][N:5]=[C:6]([C:9]1[C:14]([Cl:15])=[CH:13][C:12]([Cl:16])=[CH:11][N:10]=1)[CH2:7][NH2:8])[CH2:2][CH3:3].C(N(CC)CC)C.[F:24][C:25]([F:36])([F:35])[C:26]1[CH:34]=[CH:33][CH:32]=[CH:31][C:27]=1[C:28](Cl)=[O:29].O>ClCCl>[Cl:15][C:14]1[C:9]([C:6](=[N:5][O:4][CH2:1][CH2:2][CH3:3])[CH2:7][NH:8][C:28](=[O:29])[C:27]2[CH:31]=[CH:32][CH:33]=[CH:34][C:26]=2[C:25]([F:24])([F:35])[F:36])=[N:10][CH:11]=[C:12]([Cl:16])[CH:13]=1
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 4

HCID 962WaterHCID 8471TriethylamineHCID 675612-(Trifluoromethyl)benzoyl chlorideHCID 1180715092-amino-1-(3,5-dichloropyridin-2-yl)ethanone-O-propyloxime

生成物 1

HCID 118071572N-[2-(3,5-dichloropyridin-2-yl)-2-(propoxyimino)ethyl]-2-(trifluoromethyl)benzamide収率 87.2%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

In a solution of 151 mg of 2-amino-1-(3,5-dichloropyridin-2-yl)ethanone-O-propyloxime and 86 mg of triethylamine in 4 ml of dichloromethane, 154 mg of 2-(trifluoromethyl)benzoyl chloride was added dropwise with stirring under cooling with ice, and after the addition, the mixture was stirred at room temperature for another 2 hours. After completion of the reaction, the reaction mixture was mixed with 10 ml of water and extracted with chloroform (30 ml×1), the resulting organic layer was washed with water (10 ml×1) and dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 2:8 to 3:7) as the eluent to obtain 218 mg of the desired product as a pale yellow resinous substance.

後処理

  1. temperatureunder cooling with ice
  2. additionafter the addition
  3. stirringthe mixture was stirred at room temperature for another 2 hours
  4. customAfter completion of the reaction
  5. extractionextracted with chloroform (30 ml×1)
  6. washthe resulting organic layer was washed with water (10 ml×1)
  7. dry with materialdried over saturated aqueous sodium chloride
  8. customanhydrous sodium sulfate, and the solvent was evaporated under reduced pressure
  9. customThe resulting residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-c97955ef590e42a7aa823e60611fccb8
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434684B2

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