Hydrochloric Acid → Methyl 4-methoxybenzimidate hydrochloride

HRID 472155

反応式

HRID 472155 の反応式
[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

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 701294-Methoxybenzonitrile

生成物 1

HCID 12463133Methyl 4-methoxybenzimidate hydrochloride

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-34fa7fc0cc4b4f1d8abfbf868d16b1a0
出典データセット
uspto-grants-2014_01
特許番号
US08633208B2

関連ノート

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