Tetrahydrofuran → 6-Amino-4-methyl-beta-carboline-3-carboxylic-acid-ethylester

HRID 1085448ノート

反応式

HRID 1085448 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]([N+:20]([O-])=O)=[CH:13][CH:12]=3)=[O:5])[CH3:2].O1CCCC1>C(O)C.[C].[Pd]>[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]

参加物

5

反応物 2

HCID 8028TetrahydrofuranHCID 130373364-Methyl-6-nitro-beta-carbolin-3-carboxylic acid ethyl ester

生成物 1

HCID 130373386-Amino-4-methyl-beta-carboline-3-carboxylic-acid-ethylester収率 88.9%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒

実験手順

1.02 g of 4-methyl-6-nitro-β-carbolin-3-carboxylic acid ethyl ester is dissolved or suspended in 30 ml of ethanol and 6 ml of tetrahydrofuran and, after the addition of 150 ml of palladium-carbon (10%), is hydrogenated at 24° C. and normal pressure. Within 3.5 hours, 210 ml of hydrogen is absorbed. The solution is filtered off and the catalyst and the solvent is distilled off in vacuo. The crude product is recrystallized from methanol-chloroform. 816 mg of 6-amino-4-methyl-β-carbolin-3-carboxylic acid ethyl ester of melting point 225°-238° C. (decomposition) is obtained.

後処理

  1. customis hydrogenated at 24° C.
  2. custom210 ml of hydrogen is absorbed
  3. filtrationThe solution is filtered off
  4. distillationthe catalyst and the solvent is distilled off in vacuo
  5. customThe crude product is recrystallized from methanol-chloroform

出典と根拠

ORDレコード
ord-cc63fabfe0d3425bb62c6a0fa6ded733
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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