Dimethyl Sulfate → 1-[2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetyl]-1-methyl-2-(phenylmethylidene)hydrazine

HRID 335469

反応式

HRID 335469 の反応式
[CH2:1]([C:3]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([CH2:10][CH3:11])[C:4]=1[C:12](=[O:24])[C:13]([NH:15][N:16]=[CH:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:14])[CH3:2].[CH2:25](C(C)=O)C(C)C.[C:32](=O)([O-])[O-].[K+].[K+].S(OC)(OC)(=O)=O>O>[CH2:1]([C:3]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([CH2:10][CH3:11])[C:4]=1[C:12](=[O:24])[C:13]([N:15]([CH3:25])[N:16]=[CH:17][C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)=[O:14])[CH3:2].[CH2:1]([C:3]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([CH2:10][CH3:11])[C:4]=1[C:12](=[O:24])[C:13](=[N:15][N:16]=[CH:17][C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)[O:14][CH3:32])[CH3:2]

参加物

7

反応物 4

HCID 6497Dimethyl SulfateHCID 7909Methyl Isobutyl KetoneHCID 11430Potassium CarbonateHCID 666919781-[2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetyl]-2-(phenylmethylidene)hydrazine

生成物 2

HCID 666915621-[2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetyl]-1-methyl-2-(phenylmethylidene)hydrazineHCID 86689363methyl 2-(2,6-diethyl-4-methylphenyl)-2-oxo-N-(phenylmethylidene)ethanehydrazonate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a 100 mL volume three-necked flask, 5.0 g of 1-[2-(2,6-diethyl-4-methylphenyl)-2-oxoacetyl]-2-(phenylmethylidene)hydrazine ((40-a)-(14)-6), 31 ml of methyl isobutyl ketone, 6.43 g of potassium carbonate and 1.75 ml of dimethyl sulfate were added and the mixture was stirred at room temperature for 7.5 hours. Water was added to the reaction mixture, the organic layer was removed and then the aqueous layer was extracted with 31 ml of methyl isobutyl ketone. The organic layers were combined, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give 0.324 g of 1-[2-(2,6-diethyl-4-methylphenyl)-2-oxoacetyl]-1-methyl-2-(phenylmethylidene)hydrazine ((40-b)-(15)-5)) and 0.324 g of methyl 2-(2,6-diethyl-4-methylphenyl)-2-oxo-N-(phenylmethylidene)ethanehydrazonate (X-1).

後処理

  1. customthe organic layer was removed
  2. extractionthe aqueous layer was extracted with 31 ml of methyl isobutyl ketone
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-85d1becec7044685bfa425d5da985022
出典データセット
uspto-grants-2014_11
特許番号
US08884010B2

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