반응 #42082

ord-b5b31bbe1b2e446d94d4b4c91c35140c

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타were combined at room temperature
  2. 2
    농축After 7 minutes the reaction was concentrated
  3. 3
    workup.DISSOLUTIONdissolved in EtOAc
  4. 4
    세척before washing with water
  5. 5
    건조drying (Na2SO4)
  6. 6
    기타The concentrated residue was purified by preparative TLC (silica gel)
  7. 7
    세척eluted with EtOAc affording the title compound

실험 절차

The product of Example 1 (65 mg), THF (3 mL), MeOH (0.33 mL) and NaBH4 (9.6 mg) were combined at room temperature. After 7 minutes the reaction was concentrated and then dissolved in EtOAc before washing with water and drying (Na2SO4). The concentrated residue was purified by preparative TLC (silica gel) eluted with EtOAc affording the title compound. HPLC/MS: 515.9 (M+1), 517.9 (M+3); Rt=3.68 min.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07728141B2uspto-grants-2010_06