Hydrochloric Acid → 1,2-Bis(4-methylphenyl)ethan-1-one

HRID 1271263

反応式

HRID 1271263 の反応式
CON(C)[C:4]([C:6]1[CH:11]=[CH:10][C:9]([CH3:12])=[CH:8][CH:7]=1)=[O:5].[CH3:14][C:15]1[CH:23]=[CH:22][C:18]([CH2:19][Mg]Cl)=[CH:17][CH:16]=1.Cl>O1CCCC1.O>[C:9]1([CH3:12])[CH:10]=[CH:11][C:6]([C:4](=[O:5])[CH2:14][C:15]2[CH:23]=[CH:22][C:18]([CH3:19])=[CH:17][CH:16]=2)=[CH:7][CH:8]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 5133773N-Methoxy-N,4-dimethylbenzamideHCID 178425359HCID 178425359、化合物

生成物 1

HCID 125039001,2-Bis(4-methylphenyl)ethan-1-one収率 64.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Under an argon atmosphere, a solution of 10.40 g of N-methoxy-N-methyl-p-toluamide in 100 ml of tetrahydrofuran was ice-cooled and 4-methylbenzylmagnesium chloride (solution prepared by dissolving 10.60 g of α-chloro-p-xylene and 1.94 g of magnesium in 85 ml of tetrahydrofuran) was added dropwise. After stirring for one hour, 100 ml of 10% hydrochloric acid was slowly added. The reaction solution was diluted with water, extracted with diethyl ether, washed with water and then dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the crude crystal was washed with diisopropyl ether and then dried under reduced pressure to obtain 8.43 g of the desired compound as a colorless crystal having a melting point of 93 to 100° C.

後処理

  1. temperaturecooled
  2. extractionextracted with diethyl ether
  3. washwashed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. washthe crude crystal was washed with diisopropyl ether
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-da645eb9e0324749b0b8bb79768544e9
出典データセット
uspto-grants-2007_04
特許番号
US07205302B2

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