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Water → HCID 57927348, 화합물

HRID 889155
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HRID 889155 반응식
[CH3:1][N:2]1[C:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:5][NH:4][C:3]1=[O:13].[Br:14][CH2:15][CH2:16][CH2:17]Br.[H-].[Na+].O>CN(C)C=O.C(OCC)(=O)C>[Br:14][CH2:15][CH2:16][CH2:17][N:4]1[C:3](=[O:13])[N:2]([CH3:1])[C:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:5]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 80011,3-DibromopropaneHCID 24758Sodium hydrideHCID 30393113H-1,2,4-Triazol-3-one, 2,4-dihydro-4-methyl-5-phenyl-

생성물 1

HCID 57927348HCID 57927348, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매
HCID 8857
Ethyl Acetate
용매

실험 절차

After dissolving 4-methyl-5-phenyl-2,4-dihydro[1,2,4]triazol-3-one (CAS 50369-39-6) (500 mg) and 1,3-dibromopropane (0.87 ml) in N,N-dimethylformamide (9 ml), sodium hydride (60% in oil) (125 mg) was added and the mixture was stirred at room temperature for 6 hours. Water was added to the reaction mixture, and extraction was performed with ethyl acetate. The organic layer was washed with water and brine in that order and then dried over anhydrous magnesium sulfate. After filtration, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound (649 mg).

후처리

  1. additionwas added
  2. washThe organic layer was washed with water and brine in that order
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationAfter filtration
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-d68c2bf347574b2bac1785f445507347
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08252810B2

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