반응 #455930

ord-57cc5aa6e90246ff8c22531c040e963e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONtreated dropwise
  2. 2
    추출the product was extracted with ethyl acetate
  3. 3
    세척the organic phase was washed with water
  4. 4
    건조dried over magnesium sulphate
  5. 5
    기타After removing the solvent there

실험 절차

1.12 g of methyl 3-amino-4-(2-chloro-5-methoxy-phenoxy)-5-[2-(tetrahydro-pyran-2-yloxy)-ethoxy]-benzoate were dissolved in a mixture of toluene/pyridine (20 ml/30 ml) treated dropwise while cooling with ice with a solution of 1.05 g of 5-isopropylpyridine-2-sulphonyl chloride in toluene (30 ml) and subsequently stirred at room temperature for 24 hours. The reaction mixture was poured on to ice/3M HCl, the product was extracted with ethyl acetate and the organic phase was washed with water and dried over magnesium sulphate. After removing the solvent there was obtained the desired methyl 4-(2-chloro-5-methoxy-phenoxy)-3-(5-isopropyl-pyridine-2-sulphonylamino)-5-[2-(tetrahydro-pyran-2-yloxy)-ethoxy]-benzoate as a yellow solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06133442uspto-grants-2000_10