Water → 1-(3-Iodophenyl)-1,3-dihydro-2h-imidazol-2-one

HRID 857124ノート

反応式

HRID 857124 の反応式
CO[CH:3](OC)[CH2:4][NH:5][C:6]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([I:15])[CH:10]=1)=[O:7].O>C(O)(=O)C>[I:15][C:11]1[CH:10]=[C:9]([N:8]2[CH:3]=[CH:4][NH:5][C:6]2=[O:7])[CH:14]=[CH:13][CH:12]=1

参加物

4

反応物 2

HCID 962WaterHCID 21867194N-(2,2-Dimethoxyethyl)-N'-(3-iodophenyl)urea

生成物 1

HCID 218671801-(3-Iodophenyl)-1,3-dihydro-2h-imidazol-2-one収率 25.7%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

N(2,2-Dimethoxyethyl)-N′-(3-iodophenyl)urea (618 mg) was dissolved in acetic acid (10 ml) and water (1 ml) and the mixture was stirred at 20° C. for 17 h and then heated to 100° C. for 0.5 h. The solvent was removed under reduced pressure and the residue was dissolved in ethyl acetate. The solution was washed with NaHCO3 solution, dried and purified by chromatography on 10 g silica Bond Elut cartridge eluting with EtOAc-petroleum ether (1:7 to 1:1) to give the title compound (130 mg) LCMS RT=2.66 min.

後処理

  1. customThe solvent was removed under reduced pressure
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washThe solution was washed with NaHCO3 solution
  4. customdried
  5. custompurified by chromatography on 10 g silica Bond Elut cartridge
  6. washeluting with EtOAc-petroleum ether (1:7 to 1:1)

出典と根拠

ORDレコード
ord-3c02eb8592054997a1ceaf4816352414
出典データセット
uspto-grants-2006_12
特許番号
US07144908B2

反応ノート

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