反応 #159220

ord-d7dfebb769c74b36bc058689e0b413e0

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The reaction was partially concentrated
  2. 2
    洗浄the resulting aqueous solution was washed with ethyl acetate
  3. 3
    抽出The acidic aqueous layer was extracted twice with ethyl acetate
  4. 4
    洗浄The combined organic layers were washed with brine
  5. 5
    乾燥dried (MgSO4)
  6. 6
    濃縮concentrated

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08822430B2uspto-grants-2014_09