Sodium Iodide → 2-Iodo-4-(trifluoromethyl)phenol

HRID 16070

反応式

HRID 16070 の反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.[Na+].[I-:13]>CN(C=O)C.Cl>[I:13][C:5]1[CH:4]=[C:3]([C:2]([F:10])([F:11])[F:1])[CH:8]=[CH:7][C:6]=1[OH:9]

参加物

5

反応物 2

HCID 5238Sodium IodideHCID 678744-(Trifluoromethyl)phenol

生成物 1

HCID 115728162-Iodo-4-(trifluoromethyl)phenol収率 91.5%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 6228Dimethylformamide溶媒

実験手順

4-(trifluoromethyl)-phenol (8 g) in anhydrous DMF (80 ml) was cooled to 0° C. NaI (9.06 g) and chloroamine-T (16.1 g) was added portionwise and stirred at room temperature overnight. Then diluted with 2M HCl and extracted with ethylacetate. The organic phase was washed with sodium thiosulfate solution, dried (MgSO4) and concentrated in vacuo. The residue was purified by chromatography (silica, eluting with isohexane:ethyl acetate) to give the sub-title compound as a yellow oil (13 g).

後処理

  1. extractionextracted with ethylacetate
  2. washThe organic phase was washed with sodium thiosulfate solution
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by chromatography (silica, eluting with isohexane:ethyl acetate)

出典と根拠

ORDレコード
ord-1e2552f608414f098ff5e79320e33a6d
出典データセット
uspto-grants-2010_06
特許番号
US07737135B2

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