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

HRID 1181559노트

반응식

HRID 1181559 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ea338a6e63af43aebc95348a60140125
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07285560B2

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