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

HRID 857124노트

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HRID 857124 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
100 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-3c02eb8592054997a1ceaf4816352414
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07144908B2

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