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Hydrochloric Acid → HCID 19971591, 화합물

HRID 1762644
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반응식

HRID 1762644 반응식
[F:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][C:3]=1[O:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[F:17][C:18](I)([F:20])[F:19].Cl>CN(C)C=O.[Zn]>[F:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]([OH:7])[C:18]([F:20])([F:19])[F:17])=[CH:4][C:3]=1[O:10][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 16843TrifluoroiodomethaneHCID 1100684-Fluoro-3-phenoxybenzaldehyde

생성물 1

HCID 19971591HCID 19971591, 화합물수율 56.7%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 6228Dimethylformamide용매

실험 절차

A mixture of 2 g of 4-fluoro-3-phenoxy-benzaldehyde, 5 ml of dimethylforomamide, 2 g of electrolytic zinc and 15 ml of a solution of 13.5 mmols of trifluoromethyl iodide in dimethylformamide was ultrasonically irradiated for 15 minutes and the mixture was poured into aqueous N hydrochloric acid. The mixture was extracted with isopropyl ether and the organic phase was evaporated to dryness under reduced pressure. The residue was chromatographed over silica gel and was eluted with a 1-1 methylene chloride-hexane mixture to be obtain 1.5 g of 1-(4-fluoro-3-phenoxy-phenyl)-2,2,2-trifluoroethanol.

후처리

  1. customwas ultrasonically irradiated for 15 minutes
  2. extractionThe mixture was extracted with isopropyl ether
  3. customthe organic phase was evaporated to dryness under reduced pressure
  4. customThe residue was chromatographed over silica gel
  5. washwas eluted with a 1-1 methylene chloride-hexane mixture

출처 및 근거

ORD 기록
ord-c0c718e5affb474680fc898cff5e46ea
출처 데이터셋
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04833163

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