Hydrochloric Acid → Methyl 4-methoxybenzimidate hydrochloride

HRID 472155

반응식

HRID 472155 반응식
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[CH:5][CH:4]=1.[ClH:11].[CH3:12][OH:13]>>[ClH:11].[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:6]([C:7](=[NH:8])[O:13][CH3:12])=[CH:5][CH:4]=1

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 701294-Methoxybenzonitrile

생성물 1

HCID 12463133Methyl 4-methoxybenzimidate hydrochloride

실험 절차

4-methoxybenzonitrile (12.5 g, 91.1 mmol) was dissolved in methanol (140 mL), through this cooled (−5° C.) solution gaseous HCl was bubbled for about 3 hours. The reaction mixture was then stirred, in a closed flask, at r.t. for 24 hours. Then the excess HCl was stripped by bubbling nitrogen and the resulting solution was concentrated, the residue was taken up with TBME (100 mL) and stirred for 30 min., then filtrated and dried to provide the title product as a colourless powder 19.0 g (quantitative). C9H11NO2.HCl, MW: 201.69 1H-NMR (300 MHz, D2O) ppm: 4.20 (s, 3H), 6.9 (m, 1H); 7.65 (m, 1H); 8.40 (m, 1H).

후처리

  1. customwas bubbled for about 3 hours
  2. customby bubbling nitrogen
  3. concentrationthe resulting solution was concentrated
  4. stirringstirred for 30 min.
  5. filtrationfiltrated
  6. customdried

출처 및 근거

ORD 기록
ord-34fa7fc0cc4b4f1d8abfbf868d16b1a0
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08633208B2

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