Acetone → HCID 136127060、化合物

HRID 432057ノート

反応式

HRID 432057 の反応式
[C:1](Cl)(=[O:3])C.CO.CC(C)=[O:9].[CH3:11][O:12][N:13]=[C:14]1[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[O:16][C:15]1=NO>O>[OH:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[C:14](=[N:13][O:12][CH3:11])[C:15]([O:3][CH3:1])=[O:9]

参加物

6

反応物 4

HCID 180AcetoneHCID 887MethanolHCID 6367Acetyl chlorideHCID 178502623HCID 178502623、化合物

生成物 1

HCID 136127060HCID 136127060、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

10.5 g of acetyl chloride (0.133 mol) are added dropwise to a mixture of 100 ml of methanol and 100 ml of acetone. 10 g (0.052 mol) of benzofuran-2,3-dione 3-(O-methyl-oxime) 2-oxime are dissolved in this mixture, and the reaction mixture is then stirred at room temperature for 12 hours. The mixture is poured into water and the product is extracted with ethyl acetate. The organic phase is washed with aqueous sodium bicarbonate solution and dried over sodium sulphate, and the solvent is distilled off under reduced pressure. This gives 9 g of crude product which, according to HPLC, contains 17.7% methyl E-2-(2-hydroxyphenyl)-2-methoxyimino-acetate of log p=1.48 and 61.8% methyl Z-2-(2-hydroxyphenyl)-2-methoxyimino-acetate of log p=2.38.

後処理

  1. extractionthe product is extracted with ethyl acetate
  2. washThe organic phase is washed with aqueous sodium bicarbonate solution
  3. dry with materialdried over sodium sulphate
  4. distillationthe solvent is distilled off under reduced pressure

出典と根拠

ORDレコード
ord-fbf6226af1a948dc9ead992ae083eff2
出典データセット
uspto-grants-2003_12
特許番号
US06660872B1

反応ノート

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