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

HRID 2259385ノート

反応式

HRID 2259385 の反応式
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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol溶媒

実験手順

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 residue 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).

後処理

  1. customThe solvent was removed by distillation under reduced pressure
  2. customThe residue 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

出典と根拠

ORDレコード
ord-cc5d7d2f22364c01b188552e799b9631
出典データセット
uspto-grants-1995_12
特許番号
US05472984

反応ノート

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