Acetic Anhydride → 6-Acetamido-4-methyl-beta-carbolin-3-carboxylic acid ethyl ester

HRID 1757979ノート

反応式

HRID 1757979 の反応式
[CH2:1]([O:3][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])[CH3:2].[C:21](OC(=O)C)(=[O:23])[CH3:22]>N1C=CC=CC=1>[CH2:1]([O:3][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]([NH:20][C:21](=[O:23])[CH3:22])=[CH:13][CH:12]=3)=[O:5])[CH3:2]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 130373386-Amino-4-methyl-beta-carboline-3-carboxylic-acid-ethylester

生成物 1

HCID 130373396-Acetamido-4-methyl-beta-carbolin-3-carboxylic acid ethyl ester

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

0.6 g of 6-amino-4-methyl-β-carbolin-3-carboxylic acid ethyl ester is dissolved in 6 ml of pyridine and 1.5 ml of acetic anhydride and the whole is stirred for 16 hours at room temperature. The mixture is then stirred into 30 ml of ice water and intensely extracted with ethyl acetate. The extracts are washed until neutral with semisaturated common salt solution, dried using sodium sulphate and filtered. The solvent is distilled off in vacuo. The residue (0.78 g) is recrystallized from acetone-diisopropyl ether. 0.49 g of 6-acetamido-4-methyl-β-carbolin-3-carboxylic acid ethyl ester of melting point 273°-278° C. is obtained.

後処理

  1. extractionintensely extracted with ethyl acetate
  2. washThe extracts are washed until neutral with semisaturated common salt solution
  3. customdried
  4. filtrationfiltered
  5. distillationThe solvent is distilled off in vacuo
  6. customThe residue (0.78 g) is recrystallized from acetone-diisopropyl ether

出典と根拠

ORDレコード
ord-c76bff1860a2467385fd35cd8a0555e5
出典データセット
uspto-grants-1983_02
特許番号
US04371536

反応ノート

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