Acetic Acid → HCID 13292908, 화합물

HRID 436823노트

반응식

HRID 436823 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 13292908HCID 13292908, 화합물수율 99.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-58ccc35fef7847b69212edd02654e57c
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04028376

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