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

HRID 1069117ノート

反応式

HRID 1069117 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-ecd50686b937470e8554ed64900c4bae
出典データセット
uspto-grants-2001_06
特許番号
US06251928B1

反応ノート

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