Water → HCID 57927538、化合物

HRID 889156ノート

反応式

HRID 889156 の反応式
[C:1]1([N:7]2[CH:11]=[N:10][NH:9][C:8]2=[O:12])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Br:13][CH2:14][CH2:15][CH2:16]Br.[H-].[Na+].O>CN(C)C=O.C(OCC)(=O)C>[Br:13][CH2:14][CH2:15][CH2:16][N:9]1[C:8](=[O:12])[N:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH:11]=[N:10]1

参加物

7

反応物 4

HCID 962WaterHCID 80011,3-DibromopropaneHCID 24758Sodium hydrideHCID 2614194-Phenyl-2,4-dihydro-3H-1,2,4-triazol-3-one

生成物 1

HCID 57927538HCID 57927538、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

After dissolving 4-phenyl-2,4-dihydro[1,2,4]triazol-3-one (CAS 1008-30-6) (1.00 g) and 1,3-dibromopropane (1.89 ml) in N,N-dimethylformamide (15 ml), sodium hydride (60% in oil) (273 mg) was added and the mixture was stirred at room temperature for 4 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. The obtained solid was washed with n-heptane to obtain the title compound (840 mg).

後処理

  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
  7. washThe obtained solid was washed with n-heptane

出典と根拠

ORDレコード
ord-bb23f3e9d3914fa6884b4da41936638c
出典データセット
uspto-grants-2012_08
特許番号
US08252810B2

反応ノート

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