Methanol → 4-(Dimethylamino)-1,1-dimethoxybut-3-en-2-one

HRID 1181559

反応式

HRID 1181559 の反応式
[CH3:1][O:2][C:3]([O:7][CH3:8])(C)[CH:4]=[O:5].CO[CH:11](OC)[N:12]([CH3:14])[CH3:13].[CH3:17]O>>[CH3:13][N:12]([CH3:14])[CH:11]=[CH:17][C:4](=[O:5])[CH:3]([O:7][CH3:8])[O:2][CH3:1]

参加物

4

反応物 3

HCID 887MethanolHCID 78373Dimethylformamide dimethyl acetalHCID 75681812,2-Dimethoxypropanal

生成物 1

HCID 27821454-(Dimethylamino)-1,1-dimethoxybut-3-en-2-one収率 70%

実験手順

300 g (307 ml, 2.54 mol) of methylglyoxal dimethyl acetal (21) were stirred, at 110° C. for 4 hours (h), together with 303 g (337 ml, 2.54 mol) of N,N-dimethylformamide dimethyl acetal (17). The methanol which was formed during the reaction was removed continuously from the reaction solution by distillation. After the reaction solution had cooled down, it was extracted with heptane and the solvent was evaporated. This resulted in 303 g of crude product 22 (yield 70%), which was reacted without any further purification.

後処理

  1. customwas removed continuously from the reaction solution by distillation
  2. temperatureAfter the reaction solution had cooled down
  3. extractionit was extracted with heptane
  4. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-ea338a6e63af43aebc95348a60140125
出典データセット
uspto-grants-2007_10
特許番号
US07285560B2

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