Acetophenone → 1-[2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetyl]-2-(1-phenyl-1-ethylidene)hydrazine

HRID 335465

反応式

HRID 335465 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:17])[C:13]([NH:15][NH2:16])=[O:14])[CH3:2].C1COCC1.[C:23]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)(=O)[CH3:24]>C(O)(=O)C>[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:17])[C:13]([NH:15][N:16]=[C:23]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[CH3:24])=[O:14])[CH3:2]

参加物

5

反応物 3

HCID 7410AcetophenoneHCID 8028TetrahydrofuranHCID 569428732-(2,6-Diethyl-4-methylphenyl)-2-oxoacetohydrazide

生成物 1

HCID 866893611-[2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetyl]-2-(1-phenyl-1-ethylidene)hydrazine収率 87.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a 50 mL volume two-necked flask, 3.0 g of 2-(2,6-diethyl-4-methylphenyl)-2-oxoacetohydrazide ((12-1)-(11)-39), 20 ml of THF (anhydrous), 1.73 g of acetophenone and 780 mg of acetic acid were added under a nitrogen atmosphere, and the mixture was stirred for 6 hours under reflux. The reaction mixture was cooled to room temperature and concentrated under reduced pressure. Water was added to the residue and the resultant was extracted with t-butyl methyl ether. The organic layer was concentrated under reduced pressure and hexane was added thereto. The precipitated crystals were collected by filtration and dried to give 3.77 g of 1-[2-(2,6-diethyl-4-methylphenyl)-2-oxoacetyl]-2-(1-phenyl-1-ethylidene)hydrazine ((40-a)-(14)-7).

後処理

  1. temperatureunder reflux
  2. concentrationconcentrated under reduced pressure
  3. additionWater was added to the residue
  4. extractionthe resultant was extracted with t-butyl methyl ether
  5. concentrationThe organic layer was concentrated under reduced pressure and hexane
  6. additionwas added
  7. filtrationThe precipitated crystals were collected by filtration
  8. customdried

出典と根拠

ORDレコード
ord-1e9b6b45e51847d59ef193e706f32213
出典データセット
uspto-grants-2014_11
特許番号
US08884010B2

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