Hydrogen Bromide → 1-(N,N-dimethylamino)methyl-3-hydroxy-2-propylbenzene

HRID 1289150ノート

反応式

HRID 1289150 の反応式
[CH3:1][N:2]([CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11]C)[C:6]=1[CH2:13][CH2:14][CH3:15])[CH3:3].Br>C(O)(=O)C>[CH3:3][N:2]([CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([OH:11])[C:6]=1[CH2:13][CH2:14][CH3:15])[CH3:1]

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 13780988(3-Methoxy-2-propylbenzyl)-dimethylamine2 回

生成物 1

HCID 137809951-(N,N-dimethylamino)methyl-3-hydroxy-2-propylbenzene収率 78.9%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

The 1-(N,N-dimethylamino)methyl-3-methoxy-2-propylbenzene was then converted to the 3-hydroxy equivalent by adding the 1-(N,N-dimethylamino)methyl-3-methoxy-2-propylbenzene (238 g, 1.15 moles) to acetic acid (2.35 L) and then adding hydrobromic acid (1 L of a 48% solution). This mixture was then stirred at reflux for thirty hours. The acetic acid was removed and the residue was redissolved in ethanol. The ethanol was then removed and the residue was again redissolved in ethanol. Diethyl ether was added under a precipitate formed. Precipition was allowed to proceed overnight and the precipitate was collected by filtration to yield 216.2 grams (78.9%) of 1-(N,N-dimethylamino)methyl-3-hydroxy-2-propylbenzene hydrobromic salt.

後処理

  1. temperatureat reflux for thirty hours
  2. customThe acetic acid was removed
  3. dissolutionthe residue was redissolved in ethanol
  4. customThe ethanol was then removed
  5. dissolutionthe residue was again redissolved in ethanol
  6. additionDiethyl ether was added under a precipitate
  7. customformed
  8. filtrationthe precipitate was collected by filtration

出典と根拠

ORDレコード
ord-ae1809cf09404d4fbd715bcf4dffd244
出典データセット
uspto-grants-1998_05
特許番号
US05747517

反応ノート

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