Aniline → 4-(1-Bromo-1,1,2,3,3,3-hexafluoro-2-propyl)aniline

HRID 1824582

反応式

HRID 1824582 の反応式
S(S([O-])=O)([O-])=O.[Na+].[Na+].[NH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C(=O)([O-])O.[Na+].[Br:21][C:22]([F:31])([F:30])[C:23](Br)([F:28])[C:24]([F:27])([F:26])[F:25].C(=O)([O-])[O-].[Na+].[Na+]>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.COC(C)(C)C.O>[Br:21][C:22]([F:31])([F:30])[C:23]([C:13]1[CH:14]=[CH:15][C:10]([NH2:9])=[CH:11][CH:12]=1)([F:28])[C:24]([F:27])([F:26])[F:25]

参加物

9

反応物 5

HCID 6115AnilineHCID 10340Sodium CarbonateHCID 24489Sodium DithioniteHCID 695791,2-Dibromo-1,1,2,3,3,3-hexafluoropropaneHCID 516892Sodium Bicarbonate

生成物 1

HCID 230649694-(1-Bromo-1,1,2,3,3,3-hexafluoro-2-propyl)aniline

試薬・触媒・溶媒 3

HCID 94433Tetrabutylammonium hydrogen sulfate触媒HCID 962Water溶媒HCID 15413tert-Butyl methyl ether溶媒2 回

実験手順

First 476.74 g (2.74 mol) of sodium dithionite and then 250 g (2.68 mol) of aniline were added at room temperature to a mixture of 4000 ml of water, 1200 ml of tert-butyl methyl ether, 270.61 g (3.22 mol) of sodium hydrogencarbonate and 10.94 g of tetra-n-butylammonium hydrogensulphate. Subsequently, a solution of 998.07 g of 1,2-dibromo-1,1,2,3,3,3-hexafluoropropane in 300 ml of tert-butyl methyl ether was added dropwise at 35–40° C. and, on completion of addition, the mixture was stirred at RT for a further 18 h. If necessary, sodium carbonate was used to adjust to a pH of 5 and the organic phase was removed, dried and concentrated. The remaining residue is incipiently distilled under reduced pressure at 0.3 mbar up to an internal temperature of 100° C.

後処理

  1. customthe organic phase was removed
  2. customdried
  3. concentrationconcentrated
  4. distillationThe remaining residue is incipiently distilled under reduced pressure at 0.3 mbar up to an internal temperature of 100° C.

出典と根拠

ORDレコード
ord-60d181a79ca94b06aeedf8f6463f5cf7
出典データセット
uspto-grants-2006_05
特許番号
US07041852B2

関連ノート

読み込み中…