反応 #1166428

ord-07cf898330654647b94c44f59c5e9c74

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他When the starting material had been consumed
  2. 2
    ろ過the mixture was filtered
  3. 3
    濃縮the filtrate was concentrated under vacuum
  4. 4
    その他The residue was purified by chromatography on silica gel
  5. 5
    洗浄eluting with 90% ethyl acetate/hexane
  6. 6
    その他to obtain a product which
  7. 7
    その他was recrystallized from ethyl acetate/hexane

実験手順

A 150 mg portion of the product of Example 279 was hydrogenated on a Parr apparatus at 40 p.s.i. in 50 mL of ethanol containing 5 mL of dimethylformamide and 20 mg of 10% palladium/carbon catalyst. When the starting material had been consumed, the mixture was filtered and the filtrate was concentrated under vacuum. The residue was purified by chromatography on silica gel, eluting with 90% ethyl acetate/hexane to obtain a product which was recrystallized from ethyl acetate/hexane to produce the desired product. m.p. 109°-111°.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05550134uspto-grants-1996_08