반응 #87296

ord-bf75a23bf707431a9d54a005a006ddd1

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타quenched with 100 μL of water
  2. 2
    여과Precipitate was filtered off
  3. 3
    세척washed with ether (3×30 mL)
  4. 4
    기타was evaporated in vacuum, and residue
  5. 5
    기타was separated by column chromatography on silica (DCM-MeOH—NH4OH 100:1:0.5)

실험 절차

2-Benzylidene-3-cyclohexylamino-indan-1-one (3, BCI) (317 mg, 1 mmol) was dissolved in dry THF (15 mL) under nitrogen. Solution of LiAlH4 (76 mg, 2 mmol) in dry THF (10 mL) was added dropwise at 0° C. Solution was stirred overnight and quenched with 100 μL of water followed by 100 μL of 15% NaOH followed by 300 μL of water. Precipitate was filtered off and washed with ether (3×30 mL). Combined liquid was evaporated in vacuum, and residue was separated by column chromatography on silica (DCM-MeOH—NH4OH 100:1:0.5).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09439877B2uspto-grants-2016_09