4,4'-Dimethylbenzhydrol → HCID 18319023、化合物

HRID 1700939

反応式

HRID 1700939 の反応式
[OH:1][CH2:2][CH2:3][S:4][CH2:5][CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][C:16](=[O:21])[C:17]([F:20])([F:19])[F:18])=[CH:10][CH:9]=1.[CH3:22][C:23]1[CH:37]=[CH:36][C:26]([CH:27](O)[C:28]2[CH:33]=[CH:32][C:31]([CH3:34])=[CH:30][CH:29]=2)=[CH:25][CH:24]=1>C1(C)C=CC=CC=1.C(OCC)(=O)C.C1(C)C=CC(S(O)(=O)=O)=CC=1>[CH3:22][C:23]1[CH:37]=[CH:36][C:26]([CH:27]([C:28]2[CH:33]=[CH:32][C:31]([CH3:34])=[CH:30][CH:29]=2)[O:1][CH2:2][CH2:3][S:4][CH2:5][CH2:6][O:7][C:8]2[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][C:16](=[O:21])[C:17]([F:18])([F:19])[F:20])=[CH:10][CH:9]=2)=[CH:25][CH:24]=1

参加物

6

反応物 2

HCID 2793564,4'-DimethylbenzhydrolHCID 183189954-[4-[2-(2-Hydroxyethylthio)ethoxy]phenyl]-1,1,1-trifluoro-2-butanone

生成物 1

HCID 18319023HCID 18319023、化合物収率 94.2%

試薬・触媒・溶媒 3

HCID 6101p-Toluenesulfonic acid触媒HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 4-[4-[2-(2-hydroxyethylthio)ethoxy]phenyl]-1,1,1-trifluoro-2-butanone (1.20 g, 3.72 mmol), 4,4′-dimethylbenzhydrol (0.95 g, 4.47 mmol) and p-toluenesulfonic acid (0.035 g) in toluene (20 ml) was heated under reflux for 15 min. The cooled reaction mixture was diluted with ethyl acetate, washed with saturated sodium bicarbonate, brine and dried (magnesium sulfate). Evaporation of the solvent in vacuo and chromatography of the residue on silica gel (elution with a gradient of ethyl acetate 20-40% in hexane) gave 1.81 g (94%) of the title material as an oil.

後処理

  1. temperatureunder reflux for 15 min
  2. customThe cooled reaction mixture
  3. washwashed with saturated sodium bicarbonate, brine
  4. dry with materialdried (magnesium sulfate)
  5. customEvaporation of the solvent in vacuo and chromatography of the residue on silica gel (
  6. washelution with a gradient of ethyl acetate 20-40% in hexane)

出典と根拠

ORDレコード
ord-efd51941c86345039b38f5193b571df7
出典データセット
uspto-grants-2002_02
特許番号
US06350892B1

関連ノート

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