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

HRID 1085452노트

반응식

HRID 1085452 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2b03e3781ff5440695c0099179aa17be
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05010077

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