Iodine chloride → 5-Chloro-2-iodo-4-(trifluoromethyl)aniline

HRID 2064128

反応式

HRID 2064128 の反応式
[I:1]Cl.[Cl:3][C:4]1[CH:5]=[C:6]([CH:8]=[CH:9][C:10]=1[C:11]([F:14])([F:13])[F:12])[NH2:7].O.O.O.C([O-])(=O)C.[Na+].C(=O)(O)[O-].[Na+].S([O-])([O-])=O.[Na+].[Na+]>C(O)(=O)C>[Cl:3][C:4]1[C:10]([C:11]([F:12])([F:13])[F:14])=[CH:9][C:8]([I:1])=[C:6]([CH:5]=1)[NH2:7]

参加物

6

反応物 4

HCID 24640Iodine chlorideHCID 679623-Chloro-4-(trifluoromethyl)anilineHCID 18470521HCID 18470521、化合物HCID 23665404Sodium Acetate Trihydrate

生成物 1

HCID 593205585-Chloro-2-iodo-4-(trifluoromethyl)aniline

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Iodine monochloride (1.5 g) was added in one portion to a mixture of 3-chloro-4-trifluoromethylaniline (1.7 g), sodium acetate trihydrate (2.2 g), and acetic acid (10 ml) at room temperature. After 30 min aqueous sodium bicarbonate/sodium sulfite was added and the mixture extracted with diethyl ether. The organic phase was dried over Na2SO4, filtered and evaporated. The residue was purified by chromatography (ethyl acetate-hexane) to afford the title compound, 2.2 g.

後処理

  1. extractionthe mixture extracted with diethyl ether
  2. dry with materialThe organic phase was dried over Na2SO4
  3. filtrationfiltered
  4. customevaporated
  5. customThe residue was purified by chromatography (ethyl acetate-hexane)

出典と根拠

ORDレコード
ord-b60f57e2e4c145499e75c59bc916ea89
出典データセット
uspto-grants-2012_10
特許番号
US08288412B2

関連ノート

読み込み中…