반응 #2010713

ord-f8becba9a545439bae63fb9ff25cbb0c

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The mixture was then evaporated to half volume
  2. 2
    온도cooled to 0° C. for 15 min
  3. 3
    기타A solid precipitated
  4. 4
    여과was filtered off
  5. 5
    기타dried

실험 절차

To a solution of 2-{2-[3-(5-fluoro-pyridin-2-yl)-5-methyl-isoxazol-4-yl]-ethyl}-thiazole-5-carboxylic acid methyl ester (1.27 g, 3.66 mmol) in THF (9 mL) was added a solution of lithium hydroxide monohydrate (307 mg, 7.31 mmol) in water (9 mL) and the resulting mixture stirred at room temperature for 2 h. The mixture was then evaporated to half volume and then acidified to pH 1 with HCl (1 N) and cooled to 0° C. for 15 min. A solid precipitated and was filtered off and dried to afford the title compound (707 mg, 58%) which was obtained as an off white solid after recrystallization from ethyl acetate. MS: m/e=332.3 [M−H]−.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08178522B2uspto-grants-2012_05