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Water → 2-Bromo-4-(1-bromo-1,1,2,3,3,3-hexafluoroprop-2-yl)-6-(difluoromethoxy)aniline

HRID 70809
ノート
印刷プレビュー

反応式

HRID 70809 の反応式
[Br:1][C:2]([F:21])([F:20])[C:3]([C:9]1[CH:15]=[C:14]([O:16][CH:17]([F:19])[F:18])[C:12]([NH2:13])=[CH:11][CH:10]=1)([F:8])[C:4]([F:7])([F:6])[F:5].[Br:22]N1C(=O)CCC1=O.O.C(=O)([O-])O.[Na+]>C(O)(=O)C.C(OCC)(=O)C>[Br:22][C:11]1[CH:10]=[C:9]([C:3]([F:8])([C:4]([F:7])([F:6])[F:5])[C:2]([Br:1])([F:20])[F:21])[CH:15]=[C:14]([O:16][CH:17]([F:18])[F:19])[C:12]=1[NH2:13]
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

7

反応物 4

HCID 962WaterHCID 67184N-bromobutanimideHCID 516892Sodium BicarbonateHCID 866729674-(1-Bromo-1,1,2,3,3,3-hexafluoropropan-2-yl)-6-(difluoromethoxy)aniline

生成物 1

HCID 866729662-Bromo-4-(1-bromo-1,1,2,3,3,3-hexafluoroprop-2-yl)-6-(difluoromethoxy)aniline収率 75%

試薬・触媒・溶媒 2

HCID 176
Acetic Acid
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
70 °C

実験手順

4-(1-Bromo-1,1,2,3,3,3-hexafluoropropan-2-yl)-6-(difluoromethoxy)aniline (810 mg) was dissolved in acetic acid, added with N-bromosuccinimide (390 mg), and stirred at 70° C. for 3 hours. Water was added to the reaction solution and extraction was carried out twice using ethyl acetate. The organic phases were combined and neutralized with sodium hydrogen carbonate solution and dried over anhydrous magnesium sulfate. The drying agent was filtered off and the solvent was removed by distillation under the reduced pressure. The resulting residues were purified by column chromatography to obtain 2-bromo-4-(1-bromo-1,1,2,3,3,3-hexafluoroprop-2-yl)-6-(difluoromethoxy)aniline (730 mg, 75%).

後処理

  1. dry with materialdried over anhydrous magnesium sulfate
  2. filtrationThe drying agent was filtered off
  3. customthe solvent was removed by distillation under the reduced pressure
  4. customThe resulting residues were purified by column chromatography

出典と根拠

ORDレコード
ord-e91a105bc48d4e5cbfffa433993d5665
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822691B2

反応ノート

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