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

HRID 1623046노트

반응식

HRID 1623046 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 (3.07 ml, 2.54 mol) of methylglyoxal dimethyl acetal (21) were stirred at 110° C. for 4 ours (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-61ae3168daba4471836d74f929444277
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08778955B2

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