반응 #799599

ord-8a6356a0510f459d86a9cf54cc9f2527

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture was heated
  2. 2
    온도to reflux for 4 h
  3. 3
    기타quenched with water
  4. 4
    추출the mixture was extracted with EtOAc
  5. 5
    건조The organic phase was dried over anhydrous Na2SO4 for 1 h
  6. 6
    여과filtered
  7. 7
    농축The filtrate was concentrated in vacuo
  8. 8
    기타the residue was chromatographed with a silica gel column (eluting agent: 200:30:1 (v/v) DCM/MeOH/NH3H2O)

실험 절차

To a suspension of 5-benzyltetrahydropyrrolo[3,4-c]pyrrole-1,3(2H,3aH)-dione (3.88 g) in THF (80 mL) at −5° C. was added LiAlH4 (1.92 g) slowly. The reaction mixture was heated to reflux for 4 h, and then quenched with water, the mixture was extracted with EtOAc. The organic phase was dried over anhydrous Na2SO4 for 1 h and filtered. The filtrate was concentrated in vacuo and the residue was chromatographed with a silica gel column (eluting agent: 200:30:1 (v/v) DCM/MeOH/NH3H2O) to give the title compound as oil (2.07 g, 61.00%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09181277B2uspto-grants-2015_11