Ethanol hydrochloride → 1-(1H-inden-6-yl)-2-[2-(N,N-dimethylamino)ethoxy]ethanol hydrochloride

HRID 976543노트

반응식

HRID 976543 반응식
C([O:4][CH:5]([C:13]1[CH:21]=[C:20]2[C:16]([CH:17]=[CH:18][CH2:19]2)=[CH:15][CH:14]=1)[CH2:6][O:7][CH2:8][CH2:9][N:10]([CH3:12])[CH3:11])(=O)C.C[O-].[Na+].CO.[ClH:27].C(O)C>CO.C(O)C>[ClH:27].[CH2:19]1[C:20]2[C:16](=[CH:15][CH:14]=[C:13]([CH:5]([OH:4])[CH2:6][O:7][CH2:8][CH2:9][N:10]([CH3:11])[CH3:12])[CH:21]=2)[CH:17]=[CH:18]1

참가 물질

6

반응물 3

HCID 21887872Ethanol hydrochlorideHCID 23694274Sodium methanolate methanolHCID 543730301-acetoxy-1-(1H-inden-6-yl)-2-[2-(N,N-dimethylamino)ethoxy]ethane

생성물 1

HCID 675958831-(1H-inden-6-yl)-2-[2-(N,N-dimethylamino)ethoxy]ethanol hydrochloride

시약·촉매·용매 2

HCID 702Ethanol용매HCID 887Methanol용매

실험 절차

In 0.5 ml of methanol was dissolved 80 mg of 1-acetoxy-1-(1H-inden-6-yl)-2-[2-(N,N-dimethylamino)ethoxy]ethane. To the solution was added 80 mg of a 28% sodium methoxide-methanol solution with ice cooling. The resulting mixture was stirred at room temperature for 20 minutes. The solvent was removed by distillation under reduced pressure. The reside thus obtained was purified by column chromatography (eluant: chloroform/methanol=20/1) to obtain a yellow oily product. The oily product was dissolved in 0.1 ml of ethanol. To the solution was added 0.1 ml of a 5.9N dry hydrogen chloride-ethanol solution at room temperature. The resulting crystals were collected by filtration to obtain 20 mg of 1-(1H-inden-6-yl)-2-[2-(N,N-dimethylamino)ethoxy]ethanol hydrochloride (compound No. 298).

후처리

  1. customThe solvent was removed by distillation under reduced pressure
  2. customThe reside thus obtained
  3. customwas purified by column chromatography (eluant: chloroform/methanol=20/1)
  4. customto obtain a yellow oily product
  5. filtrationThe resulting crystals were collected by filtration

출처 및 근거

ORD 기록
ord-ac9fa80449764651884fe875ddc339f8
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05612381

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