Acetic Acid → HCID 13292908、化合物

HRID 436823ノート

反応式

HRID 436823 の反応式
[CH3:1][N:2]([CH3:15])[C:3]([NH:5][C:6]1[O:10][N:9]=[C:8]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:7]=1)=[O:4].C([O-])(=O)C.[Na+].C(O)(=O)C.[Br:25]Br>C(Cl)Cl>[CH3:1][N:2]([CH3:15])[C:3]([NH:5][C:6]1[O:10][N:9]=[C:8]([C:11]([CH3:12])([CH3:14])[CH3:13])[C:7]=1[Br:25])=[O:4]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 24408BromineHCID 517045Sodium AcetateHCID 132928951,1-Dimethyl-3-(5-tert-butyl-4-isoxazolyl)urea

生成物 1

HCID 13292908HCID 13292908、化合物収率 99.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a mixture of 1,1-dimethyl-(3-t-butyl-5-isoxazolyl)-urea (0.70 g), anhydrous sodium acetate (0.30 g) and glacial acetic acid (3.3 ml), bromine (0.53 g) is added dropwise in 10 minutes with ice cooling and stirring and the resultant mixture is stirred for 15 minutes. The reaction mixture is poured into ice water (30 ml) and shaken with methylene chloride. The organic layer is washed with saturated aqueous sodium bicarbonate solution and then water and evaporated to remove the solvent. The residue is recrystallized from benzene to give 1,1-dimethyl-3-(3-t-butyl-4-bromo-5-isoxazolyl)urea (0.96 g) as crystals melting at 175.5° to 176.5° C. (decomp.).

後処理

  1. additionis added dropwise in 10 minutes with ice cooling
  2. washThe organic layer is washed with saturated aqueous sodium bicarbonate solution
  3. customwater and evaporated
  4. customto remove the solvent
  5. customThe residue is recrystallized from benzene

出典と根拠

ORDレコード
ord-58ccc35fef7847b69212edd02654e57c
出典データセット
uspto-grants-1977_06
特許番号
US04028376

反応ノート

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