반응 #44614

ord-06216df421d042e5a78da4bf596942dd

반응 조건

온도
-15°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The resulting reaction solution
  2. 2
    workup.STIRRINGThe resulting mixture was stirred at room temperature for 30 min
  3. 3
    여과filtered through Celite
  4. 4
    농축The filtrate was concentrated under reduced pressure

실험 절차

LAH (483 mg) was added to a THF solution (50 mL) of (2R,5S)-5-(3,4,5-trifluorophenyl)pyrrolidine-2-carboxylic acid ethyl ester (2.91 g) over 1 hr at −15° C. The resulting reaction solution was stirred at −15° C. for 19 hr. To the reaction solution, water (0.5 mL), a 5 N sodium hydroxide aqueous solution (0.5 mL), and water (1.5 mL) were added in this order. The resulting mixture was stirred at room temperature for 30 min and then filtered through Celite. The filtrate was concentrated under reduced pressure to give 2.4 g of the title compound. The physical property values of this compound were as follows:

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07737141B2uspto-grants-2010_06