반응 #159220

ord-d7dfebb769c74b36bc058689e0b413e0

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The reaction was partially concentrated
  2. 2
    세척the resulting aqueous solution was washed with ethyl acetate
  3. 3
    추출The acidic aqueous layer was extracted twice with ethyl acetate
  4. 4
    세척The combined organic layers were washed with brine
  5. 5
    건조dried (MgSO4)
  6. 6
    농축concentrated

실험 절차

To a solution of 6-(2-methoxycarbonylamino-3-methyl-butyryl)-5-oxa-6-aza-spiro[3.4]octane-7-carboxylic acid ethyl ester (1.31 g, 3.83 mmol) in ethanol (10 mL) was added a solution of lithium hydroxide (1M in water, 7.6 mL, 7.6 mmol). The reaction was stirred at room temperature for 30 minutes. The reaction was partially concentrated and the resulting aqueous solution was washed with ethyl acetate. The ethyl acetate layer was discarded and the aqueous layer was acidified using concentrated HCl. The acidic aqueous layer was extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried (MgSO4) and concentrated to yield crude 6-(2-methoxycarbonylamino-3-methyl-butyryl)-5-oxa-6-aza-spiro[3.4]octane-7-carboxylic acid, which was used without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08822430B2uspto-grants-2014_09