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Hydrochloric Acid → HCID 19971591、化合物

HRID 1762644
ノート
印刷プレビュー

反応式

HRID 1762644 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 19971591HCID 19971591、化合物収率 56.7%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c0c718e5affb474680fc898cff5e46ea
出典データセット
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04833163

反応ノート

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