HCID 20148433、化合物 → HCID 13315116、化合物

HRID 569027ノート

反応式

HRID 569027 の反応式
[N:1]1([C:7]2[CH:8]=[C:9]3[C:17](=[CH:18][CH:19]=2)[NH:16][C:15]2[CH:14]=[N:13][C:12](C(O)=O)=[C:11]([CH3:23])[C:10]3=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1>N1C2C(=CC=CC=2)C=CC=1.[Cu]>[N:1]1([C:7]2[CH:8]=[C:9]3[C:17](=[CH:18][CH:19]=2)[NH:16][C:15]2[CH:14]=[N:13][CH:12]=[C:11]([CH3:23])[C:10]3=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

参加物

4

反応物 1

HCID 20148433HCID 20148433、化合物

生成物 1

HCID 13315116HCID 13315116、化合物収率 32.2%

試薬・触媒・溶媒 2

HCID 23978Copper触媒HCID 7047Quinoline溶媒

実験手順

2.5 g of 6-piperidino-4-methyl-β-carboline-3-carboxylic acid are heated with 520 mg of copper powder in 50 ml of quinoline for 1.5 hours to 190°-220° C. bath temperature. After distilling off the quinoline in a bulb tube, it is dispersed in ethyl acetate/10% aqueous ammonia. The precipitate that is formed is filtered off and absorptively precipated with ethanol. The combined evaporation residue of the ethanol extraction and the ethyl acetate phase yields 690 mg of 6-piperidino-4-methyl-β-carboline with a 235°-238° C. (decomposition) melting point by crystallization from ethylacetate/diisopropylether.

後処理

  1. distillationAfter distilling off the quinoline in a bulb tube
  2. additionit is dispersed in ethyl acetate/10% aqueous ammonia
  3. customThe precipitate that is formed
  4. filtrationis filtered off and absorptively precipated with ethanol
  5. customThe combined evaporation residue of the ethanol extraction

出典と根拠

ORDレコード
ord-8a42dd8bae574832a6a9bfa66373b0b3
出典データセット
uspto-grants-1988_03
特許番号
US04731358

反応ノート

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