1H-Imidazole, 2-(1-methylethyl)- → 1-(4-Imidazolylsulfonyl)-2-isopropylimidazole

HRID 1580105노트

반응식

HRID 1580105 반응식
[NH:1]1[CH:5]=[C:4]([S:6](Cl)(=[O:8])=[O:7])[N:3]=[CH:2]1.[CH:10]([C:13]1[NH:14][CH:15]=[CH:16][N:17]=1)([CH3:12])[CH3:11]>C1COCC1>[NH:1]1[CH:5]=[C:4]([S:6]([N:14]2[CH:15]=[CH:16][N:17]=[C:13]2[CH:10]([CH3:12])[CH3:11])(=[O:8])=[O:7])[N:3]=[CH:2]1

참가 물질

4

반응물 2

HCID 1234571H-Imidazole, 2-(1-methylethyl)-HCID 178527435HCID 178527435, 화합물

생성물 1

HCID 1784401171-(4-Imidazolylsulfonyl)-2-isopropylimidazole

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A round bottom flask equipped with a magnetic stirrer, reflux condenser and nitrogen inlet was charged with 8.35 g of imidazole-4-sulfonylchloride and 150 ml of THF. This solution was treated with 11.10 g of 2-isopropylimidazole in one portion and the solution stirred 24 hours at room temperature. The solution was concentrated to a clear oil and partitioned between ethylacetate and water. The organic layer was washed with water and the water washes back extracted with ethyl acetate. The organic layer was dried (Na2SO4) and concentrated to a foam. The foam was dissolved in acetone and chromatographed on activity III alumina to separate 1-(4-imidazolylsulfonyl)-2-isopropylimidazole, mp 118°-120°.

후처리

  1. customA round bottom flask equipped with a magnetic stirrer
  2. temperaturereflux condenser and nitrogen inlet
  3. concentrationThe solution was concentrated to a clear oil
  4. custompartitioned between ethylacetate and water
  5. washThe organic layer was washed with water
  6. extractionthe water washes back extracted with ethyl acetate
  7. dry with materialThe organic layer was dried (Na2SO4)
  8. concentrationconcentrated to a foam
  9. dissolutionThe foam was dissolved in acetone
  10. customchromatographed on activity III alumina
  11. customto separate 1-(4-imidazolylsulfonyl)-2-isopropylimidazole, mp 118°-120°

출처 및 근거

ORD 기록
ord-b6530124932e4f42a00c3876472dab12
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03932444

반응 노트

불러오는 중…