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

HRID 16070

반응식

HRID 16070 반응식
[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]

참가 물질

5

반응물 2

HCID 5238Sodium IodideHCID 678744-(Trifluoromethyl)phenol

생성물 1

HCID 115728162-Iodo-4-(trifluoromethyl)phenol수율 91.5%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-1e2552f608414f098ff5e79320e33a6d
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737135B2

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