Methanol → Methyl 1-methyl-4,5-dihydro-1H-imidazole-4-carboxylate

HRID 1721823노트

반응식

HRID 1721823 반응식
Cl.[CH3:2][N:3]1[CH2:7][CH:6]([C:8]([OH:10])=[O:9])[N:5]=[CH:4]1.[CH3:11]O>>[CH3:2][N:3]1[CH2:7][CH:6]([C:8]([O:10][CH3:11])=[O:9])[N:5]=[CH:4]1

참가 물질

3

실험 절차

17.0 g of 38C was dissolved in 203 ml of anhydrous methanol and dry hydrogen chloride was bubbled rapidly into the mixture while it was heated to and at reflux for 2 hours. the mixture was cooled, stripped of volatiles, mixed with 300 ml of water, neutralized with solid sodium bicarbonate, made basic to pH=9 with 3N aqueous sodium carbonate solution. The aqueous phase was extracted with methylene chloride, the extract was dried (MgSO4), filtered and stripped of solvent, to give methyl 1-methylimidazoline-4-carboxylate (38D), as a brown oil.

후처리

  1. customdry hydrogen chloride was bubbled rapidly into the mixture while it
  2. temperaturewas heated to and
  3. temperatureat reflux for 2 hours
  4. temperaturethe mixture was cooled
  5. additionmixed with 300 ml of water
  6. extractionThe aqueous phase was extracted with methylene chloride
  7. dry with materialthe extract was dried (MgSO4)
  8. filtrationfiltered

출처 및 근거

ORD 기록
ord-c4ee0e43f02a490fb709b474d23e6804
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04853027

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