Ethyl Acetate → HCID 59150509、化合物

HRID 1668588ノート

反応式

HRID 1668588 の反応式
[CH3:1][N:2]1[C:6]([C:7]2[CH:16]=[CH:15][CH:14]=[C:13]3[C:8]=2[CH:9]=[CH:10][C:11]([CH3:17])=[N:12]3)=[N:5][NH:4][C:3]1=[S:18].Br[CH2:20][CH2:21][CH2:22][CH2:23][Cl:24].[H-].[Na+].C(OCC)(=O)C>CCO>[Cl:24][CH2:23][CH2:22][CH2:21][CH2:20][S:18][C:3]1[N:2]([CH3:1])[C:6]([C:7]2[CH:16]=[CH:15][CH:14]=[C:13]3[C:8]=2[CH:9]=[CH:10][C:11]([CH3:17])=[N:12]3)=[N:5][N:4]=1

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 24758Sodium hydrideHCID 813641-Bromo-4-chlorobutaneHCID 446275704-methyl-5-(2-methyl-5-quinolinyl)-4H-1,2,4-triazole-3-thiol

生成物 1

HCID 59150509HCID 59150509、化合物収率 79%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

4-Methyl-5-(2-methyl-5-quinolinyl)-2,4-dihydro-3H-1,2,4-triazole-3-thione (400 mg) was reacted with 1-bromo-4-chloro-butane (0.233 ml) and NaH (60%, 69 mg) in absolute EtOH (6.5 ml) at reflux for 45 min. Ethyl acetate was added, the insoluble salts were filtered off and the solvent was evaporated under reduced pressure. The crude was purified on silica gel (eluent: ethyl acetate to ethyl acetate/acetone, 1/1) affording the desired compound as pale yellow solid (430 mg, 79% yield).

後処理

  1. temperatureat reflux for 45 min
  2. filtrationthe insoluble salts were filtered off
  3. customthe solvent was evaporated under reduced pressure
  4. customThe crude was purified on silica gel (eluent: ethyl acetate to ethyl acetate/acetone, 1/1)

出典と根拠

ORDレコード
ord-d4e499fc50cb4a8da9aef7d70c2a7594
出典データセット
uspto-grants-2011_08
特許番号
US07989444B2

反応ノート

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