Bromine → 5-Bromo-2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxol

HRID 37570ノート

反応式

HRID 37570 の反応式
[Cl:1][CH:2]([C:7]1([C:16]([F:19])([F:18])[F:17])[O:11][C:10]2[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=2[O:8]1)[C:3]([F:6])([F:5])[F:4].[Br:20]Br>C(Cl)(Cl)(Cl)Cl>[Br:20][C:13]1[CH:14]=[CH:15][C:9]2[O:8][C:7]([CH:2]([Cl:1])[C:3]([F:6])([F:5])[F:4])([C:16]([F:19])([F:18])[F:17])[O:11][C:10]=2[CH:12]=1

参加物

4

反応物 2

HCID 24408BromineHCID 544550482-(1-Chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole

生成物 1

HCID 189959465-Bromo-2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxol

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

51 g of 2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole from Example 2 or 17 were dissolved in 300 ml of carbon tetrachloride, and 0.5 g of anhydrous FeCl3 was added. 32 g of bromine were then added and the mixture was stirred for 3 hours under reflux. After cooling, it was washed with 10% NaHSO3 solution, dried over MgSO4 and distilled. The yield was 49 g (63% of theory) and the boiling point was 94°-98° C. at 8 mbar.

後処理

  1. temperatureunder reflux
  2. temperatureAfter cooling
  3. washit was washed with 10% NaHSO3 solution
  4. dry with materialdried over MgSO4
  5. distillationdistilled

出典と根拠

ORDレコード
ord-1eba8ac17a194999a5a00ec607a7f37b
出典データセット
uspto-grants-1995_05
特許番号
US05420309

反応ノート

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