Lithium Hydroxide → 6-(2-Methoxycarbonylamino-3-methyl-butyryl)-5-oxa-6-aza-spiro[3.4]octane-7-carboxylic acid
反応式
C([O:3][C:4]([CH:6]1[CH2:13][C:9]2([CH2:12][CH2:11][CH2:10]2)[O:8][N:7]1[C:14](=[O:24])[CH:15]([NH:19][C:20]([O:22][CH3:23])=[O:21])[CH:16]([CH3:18])[CH3:17])=[O:5])C.[OH-].[Li+]>C(O)C>[CH3:23][O:22][C:20]([NH:19][CH:15]([CH:16]([CH3:18])[CH3:17])[C:14]([N:7]1[CH:6]([C:4]([OH:5])=[O:3])[CH2:13][C:9]2([CH2:12][CH2:11][CH2:10]2)[O:8]1)=[O:24])=[O:21]参加物
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.
後処理
- concentrationThe reaction was partially concentrated
- washthe resulting aqueous solution was washed with ethyl acetate
- extractionThe acidic aqueous layer was extracted twice with ethyl acetate
- washThe combined organic layers were washed with brine
- dry with materialdried (MgSO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-fbeb6ddeecd64a2ab6b0c6630fd678c4
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08841278B2
反応ノート
読み込み中…