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

HRID 1085449노트

반응식

HRID 1085449 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1febac9703384ab9b83da4eba06571fd
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05010077

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