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

Dimethylformamide → 2-Bromo-4-(1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl)-6-(trifluoromethyl)benzenamine

HRID 2360361
ノート
印刷プレビュー

反応式

HRID 2360361 の反応式
[F:1][C:2]([F:21])([F:20])[C:3]([F:19])([C:8]1[CH:14]=[CH:13][C:11]([NH2:12])=[C:10]([C:15]([F:18])([F:17])[F:16])[CH:9]=1)[C:4]([F:7])([F:6])[F:5].CN(C=O)C.[Br:27]N1C(=O)CCC1=O>O>[Br:27][C:13]1[CH:14]=[C:8]([C:3]([F:19])([C:4]([F:7])([F:6])[F:5])[C:2]([F:20])([F:21])[F:1])[CH:9]=[C:10]([C:15]([F:16])([F:17])[F:18])[C:11]=1[NH2:12]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 67184N-bromobutanimideHCID 582974594-[1,2,2,2-Tetrafluoro-1-(trifluoromethyl)ethyl]-2-(trifluoromethyl)benzenamine

生成物 1

HCID 582975582-Bromo-4-(1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl)-6-(trifluoromethyl)benzenamine収率 80%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

100 g (0.273 mol) of 4-(perfluoropropan-2-yl)-2-(trifluoromethyl)aniline was charged to 500 ml of DMF, and 52.1 g (0.287 mol) of N-bromosuccinimide was charged in separate portions thereto over 30 minutes. After stirring at 60° C. for 2 hours, and then cooling to room temperature, the mixture was discharged to 2000 ml of water. The mixture was extracted with ethyl acetate, then washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the obtained residue was purified by silica gel column chromatography (eluent solvent; hexane:ethyl acetate=20:1) to prepare 89.0 g (yield 80%) of a target compound.

後処理

  1. additionwas charged in separate portions
  2. temperaturecooling to room temperature
  3. extractionThe mixture was extracted with ethyl acetate
  4. washwashed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customthe obtained residue was purified by silica gel column chromatography (eluent solvent; hexane:ethyl acetate=20:1)

出典と根拠

ORDレコード
ord-f4779b8b469549c8acf218e64c4e2860
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08686044B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート