반응 #436162

ord-6369df8879ef40acb2b705505c22d39c

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축then concentrated under reduced pressure
  2. 2
    workup.ADDITIONThe residue was diluted with water
  3. 3
    세척washed with ethyl acetate
  4. 4
    추출extracted with chloroform (4×100 mL)
  5. 5
    건조The combined organic extracts were dried (sodium sulfate)
  6. 6
    여과filtered
  7. 7
    농축concentrated under reduced pressure

실험 절차

To a stirred solution of Methyl 4-butyl-8-(1,3-oxazol-2-yl)-3,4-dihydro-2H-1,4-benzoxazine-6-carboxylate (474 mg) in methanol (20 mL) was added potassium hydroxide (15 mL of a 1.0 M solution in water). The mixture was stirred at room temperature overnight then concentrated under reduced pressure. The residue was diluted with water and washed with ethyl acetate. The aqueous layer was acidified to pH 4 with 1 N hydrochloric acid and extracted with chloroform (4×100 mL). The combined organic extracts were dried (sodium sulfate), filtered, and concentrated under reduced pressure to give 450 mg of the title compound: 1H NMR (300 MHz, CDCl3) δ 11.60, 8.08, 7.74, 7.46, 7.37, 4.46, 3.43, 3.34, 1.62, 1.41, 0.98.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07176242B2uspto-grants-2007_02