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

HRID 1289150노트

반응식

HRID 1289150 반응식
[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]

참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 13780988(3-Methoxy-2-propylbenzyl)-dimethylamine2회

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ae1809cf09404d4fbd715bcf4dffd244
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05747517

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