3-Methoxyacetophenone → 2-(1-Isopropyl-2-pyrrolidinylidene)-1-(3-methoxyphenyl)ethanone

HRID 2049652ノート

反応式

HRID 2049652 の反応式
[Na].COS([O-])(=O)=O.[CH:8]([N+:11]1[CH2:15][CH2:14][CH2:13][C:12]=1N(C)C)([CH3:10])[CH3:9].[CH3:19][C:20]([C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([O:28][CH3:29])[CH:23]=1)=[O:21]>C(O)C>[CH:8]([N:11]1[CH2:15][CH2:14][CH2:13][C:12]1=[CH:19][C:20]([C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([O:28][CH3:29])[CH:23]=1)=[O:21])([CH3:10])[CH3:9]

参加物

5

反応物 3

HCID 114603-MethoxyacetophenoneHCID 5360545SodiumHCID 1784564382-Dimethylamino-1-isopropyl-1-pyrrolinium methyl sulfate

生成物 1

HCID 572107862-(1-Isopropyl-2-pyrrolidinylidene)-1-(3-methoxyphenyl)ethanone

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 7.6 g of sodium in 100 ml of ethanol is added dropwise(*) at 90° within 2 hours to a mixture of 88 g of 1-isopropyl-2-dimethylamino-1-pyrrolinium methyl sulfate and 42 g of 3-methoxyacetophenone. Stirring is continued for a further 4 hours at this temperature; the solvent is distilled off in a vacuum; and the residue is distributed in 250 ml of dichloromethane and 250 ml of water. The organic phase is collected, dried over sodium sulfate and concentrated. The oil remaining behind is freed from excess 3-methoxyacetophenone by heating under a high vacuum. Yield: 42.8 g (59% of theory) of the title compound as brown oil.

後処理

  1. distillationthe solvent is distilled off in a vacuum
  2. customThe organic phase is collected
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. temperatureby heating under a high vacuum

出典と根拠

ORDレコード
ord-67bb16cf2b7143e99d59240f1d062cf5
出典データセット
uspto-grants-1980_04
特許番号
US04198424

反応ノート

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