Sodium Hydroxide → HCID 57268046、化合物

HRID 365348ノート

反応式

HRID 365348 の反応式
[OH-].[Na+].[CH:3]([O:6][C:7]([C:9]1[N:10]=[CH:11][C:12]2[NH:13][C:14]3[C:19]([C:20]=2[C:21]=1[CH2:22][CH3:23])=[CH:18][C:17]([NH:24][C:25](=[S:27])[CH3:26])=[CH:16][CH:15]=3)=[O:8])([CH3:5])[CH3:4]>O.N1C=CC=CC=1.C(OCC)(=O)C>[CH:3]([O:6][C:7]([C:9]1[N:10]=[CH:11][C:12]2[NH:13][C:14]3[C:19]([C:20]=2[C:21]=1[CH2:22][CH3:23])=[C:18]1[S:27][C:25]([CH3:26])=[N:24][C:17]1=[CH:16][CH:15]=3)=[O:8])([CH3:5])[CH3:4]

参加物

6

反応物 2

HCID 14798Sodium HydroxideHCID 53883802HCID 53883802、化合物

生成物 1

HCID 57268046HCID 57268046、化合物収率 15.1%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 1049Pyridine溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
4 °C

実験手順

450 mg of K3Fe(CN)6 is dissolved in 1.8 ml of water, mixed with 1.4 ml of 1N NaOH and cooled to 4° C. 200 mg of 4-ethyl-6-thioacetylamino-β-carboline-3-carboxylic acid isopropyl ester in 4 ml of pyridine is added in drops to this solution and stirred for another 2 hours at this temperature. The reaction mixture is taken up in ethyl acetate, washed with water, dried and concentrated by evaporation. The residue is chromatographed on silica gel with toluene+ethanol=95+5. The desired fractions are concentrated by evaporation and stirred up with ether. 30 mg of the title compound with a melting point of 239-240° C. is obtained.

後処理

  1. washwashed with water
  2. customdried
  3. concentrationconcentrated by evaporation
  4. customThe residue is chromatographed on silica gel with toluene+ethanol=95+5
  5. concentrationThe desired fractions are concentrated by evaporation
  6. stirringstirred up with ether

出典と根拠

ORDレコード
ord-0d8760b0e1f34d91958b7f6941cb1d53
出典データセット
uspto-grants-2000_10
特許番号
US06127368

反応ノート

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