Dimethylamine → 6-amino-4-methyl-beta-carbolin-3-carboxylic acid N,N-dimethylamide

HRID 1085452ノート

反応式

HRID 1085452 の反応式
C(O[C:4]([C:6]1[N:7]=[CH:8][C:9]2[NH:10][C:11]3[C:16]([C:17]=2[C:18]=1[CH3:19])=[CH:15][C:14]([NH2:20])=[CH:13][CH:12]=3)=[O:5])C.[CH3:21][NH:22][CH3:23]>C(O)CO>[CH3:21][N:22]([CH3:23])[C:4]([C:6]1[N:7]=[CH:8][C:9]2[NH:10][C:11]3[C:16]([C:17]=2[C:18]=1[CH3:19])=[CH:15][C:14]([NH2:20])=[CH:13][CH:12]=3)=[O:5]

参加物

4

反応物 2

HCID 674DimethylamineHCID 130373386-Amino-4-methyl-beta-carboline-3-carboxylic-acid-ethylester

生成物 1

HCID 130373556-amino-4-methyl-beta-carbolin-3-carboxylic acid N,N-dimethylamide

試薬・触媒・溶媒 1

HCID 174Ethylene Glycol溶媒

反応条件

温度
100 °C

実験手順

0.3 g of 6-amino-4-methyl-β-carbolin-3-carboxylic acid ethyl ester is suspended in 5 ml of ethylene glycol and, after the addition of 3 ml of dimethylamine, the whole is heated for 22 hours at 100° C. After cooling, the mixture is poured into 30 ml of ice water, extracted with ethyl acetate, washed with water until neutral, dried using sodium sulphate, filtered and the solvent is distilled off in vacuo. The crude product precipitates as a fine brown powder. 0.2 g of 6-amino-4-methyl-β-carbolin-3-carboxylic acid N,N-dimethylamide of melting point 235°-245° C. (decomposition) is obtained.

後処理

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. washwashed with water until neutral,
  4. customdried
  5. filtrationfiltered
  6. distillationthe solvent is distilled off in vacuo
  7. customThe crude product precipitates as a fine brown powder

出典と根拠

ORDレコード
ord-2b03e3781ff5440695c0099179aa17be
出典データセット
uspto-grants-1991_04
特許番号
US05010077

反応ノート

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