N-(2-aminoethyl)acetamide → HCID 19036526、化合物

HRID 264542

反応式

HRID 264542 の反応式
O=[CH:2][CH2:3][CH:4]1[CH2:13][CH2:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[O:14][CH3:15])[C:5]1=O.[C:17]([NH:20][CH2:21][CH2:22][NH2:23])(=[O:19])[CH3:18]>C(O)(=O)C>[CH3:15][O:14][C:10]1[C:11]2[CH2:12][CH2:13][C:4]3[CH:3]=[CH:2][N:23]([CH2:22][CH2:21][NH:20][C:17](=[O:19])[CH3:18])[C:5]=3[C:6]=2[CH:7]=[CH:8][CH:9]=1

参加物

4

反応物 2

HCID 66082N-(2-aminoethyl)acetamideHCID 190363722-(2-Oxoethyl)-5-methoxy-1-tetralone

生成物 1

HCID 19036526HCID 19036526、化合物収率 46%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

175 mg of 2-(2-oxoethyl)-5-methoxy-1-tetralone and 144 mg of N-acetylethylenediamine were heated to reflux under argon in 4 ml of acetic acid for 1.5 hours. The solvent was removed in a vacuum. The residue was taken up in 25 ml of water and extracted several times with dichloromethane. Chromatography on 20 g of silica gel with ethyl acetate gave a greenish coloured oil. This was crystallized from toluene for purification. 91 mg (46%) of N-[2-(4,5-dihydro-6-methoxy-1H-benz[g]indol-1-yl)ethyl]-acetamide with m.p. 133° were obtained.

後処理

  1. customThe solvent was removed in a vacuum
  2. extractionextracted several times with dichloromethane
  3. customChromatography on 20 g of silica gel with ethyl acetate gave a greenish coloured oil
  4. customThis was crystallized from toluene for purification

出典と根拠

ORDレコード
ord-6e8467599f374d0a8bc719705f2a54b4
出典データセット
uspto-grants-1997_07
特許番号
US05646173

関連ノート

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