Ethyl Acetate → HCID 59150509, 화합물

HRID 1668588노트

반응식

HRID 1668588 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 59150509HCID 59150509, 화합물수율 79%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-d4e499fc50cb4a8da9aef7d70c2a7594
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07989444B2

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