Dimethylformamide dimethyl acetal → 1-Penten-3-one, 1-(dimethylamino)-4,4-dimethoxy-

HRID 1623045ノート

反応式

HRID 1623045 の反応式
[CH3:1][O:2][C:3]([O:8][CH3:9])([CH3:7])[C:4](=[O:6])[CH3:5].CO[CH:12](OC)[N:13]([CH3:15])[CH3:14]>CO>[CH3:12][N:13]([CH3:15])[CH:14]=[CH:5][C:4](=[O:6])[C:3]([O:8][CH3:9])([O:2][CH3:1])[CH3:7]

参加物

4

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 1408713,3-Dimethoxy-2-butanone

生成物 1

HCID 5668111-Penten-3-one, 1-(dimethylamino)-4,4-dimethoxy-収率 90.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

100 g (0.76 mol) of 3,3-dimethoxy-2-butanone (16) were stirred together with 90.2 g of N,N-dimethylformamide dimethyl acetal (17) (0.76 mol) at 120° C. for 48 h. The methanol which was formed in the reaction was removed continuously from the reaction solution by means of distillation. Crystallization occurred spontaneously when the solution was cooled, with the crystallization being brought to completion by adding a little heptane. This resulted in 128.24 g of crude product 18 (yield 90%), which was reacted without any further purification.

後処理

  1. customwas removed continuously from the reaction solution by means of distillation
  2. customCrystallization
  3. temperaturewas cooled, with the crystallization
  4. additionby adding a little heptane

出典と根拠

ORDレコード
ord-825c72230d9c43feac0c79a4a2c44c21
出典データセット
uspto-grants-2014_07
特許番号
US08778955B2

反応ノート

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