반응 #2488536

ord-e0c822f7c1c744e0a75bd1d1f0411938

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The vial was sealed
  2. 2
    추출The aqueous was extracted with EtOAc
  3. 3
    세척the combined layers washed with brine
  4. 4
    건조dried over Na2SO4
  5. 5
    여과filtered
  6. 6
    농축concentrated

실험 절차

To a resealable vial was added 4-(2-(4-chlorobenzoyl)phenyl)-5-methylisoxazole-3-carbaldehyde from Example 15 (0.100 g, 0.307 mmol) and THF (2.0 mL). The vial was sealed and cooled to −78° C. before addition of methylmagnesium chloride (0.107 mL, 0.322 mmol). The reaction was stirred at −78° C. for 30 min before addition of ammonium chloride solution and water. The aqueous was extracted with EtOAc and the combined layers washed with brine, dried over Na2SO4, filtered, and concentrated to afford crude (4-chlorophenyl)(2-(3-(1-hydroxyethyl)-5-methylisoxazol-4-yl)phenyl)methanone (0.092 g, 0.269 mmol).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08796261B2uspto-grants-2014_08