Ethylbenzene → 4'-Ethylbenzoin

HRID 375038

反応式

HRID 375038 の反応式
O.[C:2]1([C:8]([CH:10]=[O:11])=[O:9])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH3:13]>ClC(Cl)C.[Ti](Cl)(Cl)(Cl)Cl>[CH2:12]([C:14]1[CH:19]=[CH:18][C:17]([CH:10]([OH:11])[C:8](=[O:9])[C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[CH:16][CH:15]=1)[CH3:13]

参加物

5

反応物 2

HCID 7500EthylbenzeneHCID 12215922Glyoxal, phenyl-, hydrate

生成物 1

HCID 153006894'-Ethylbenzoin収率 74%

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒HCID 63651,1-Dichloroethane溶媒

実験手順

Phenylglyoxal monohydrate (304 mg, 2 mM) and ethylbenzene (0.49 ml, 4 mM) were dissolved in dichloroethane (4 ml), titanium tetrachloride (0.33 ml, 3 mM) was added, and reacted at room temperature for 2 hours. The reaction mixture was extracted with ethylacetate, the extract was washed with saturated sodium hydrogen carbonate solution and brine, dried with sodium sulfate anhydrous, and then concentrated to obtain a yellow-colored oil. The oil was crystallized from a petroleum ether/diethylether to obtain 357.1 mg (74.0% yield) of 4'-ethylbenzoin.

後処理

  1. customreacted at room temperature for 2 hours
  2. extractionThe reaction mixture was extracted with ethylacetate
  3. washthe extract was washed with saturated sodium hydrogen carbonate solution and brine
  4. dry with materialdried with sodium sulfate anhydrous
  5. concentrationconcentrated
  6. customto obtain a yellow-colored oil
  7. customThe oil was crystallized from a petroleum ether/diethylether

出典と根拠

ORDレコード
ord-374784cfa61e419b83146e90f4f0eb8b
出典データセット
uspto-grants-1996_01
特許番号
US05484689

関連ノート

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