反応式
C([O:3][C:4]([C:6]1([CH3:21])[CH2:9][CH2:8][N:7]1[C:10](=[O:20])[CH2:11][C:12]1[CH:17]=[C:16]([CH3:18])[CH:15]=[C:14]([CH3:19])[CH:13]=1)=[O:5])C.CCO.[OH-].[Na+]>CO>[CH3:19][C:14]1[CH:13]=[C:12]([CH2:11][C:10]([N:7]2[CH2:8][CH2:9][C:6]2([CH3:21])[C:4]([OH:5])=[O:3])=[O:20])[CH:17]=[C:16]([CH3:18])[CH:15]=1参加物
5
反応条件
- 温度
- 20 °C
実験手順
To a solution of 1-[2-(3,5-dimethyl-phenyl)-acetyl]-2-methyl-azetidine-2-carboxylic acid ethyl ester, Intermediate 94 (1 eq.) in either EtOH or MeOH was added aqueous NaOH (2N) (2 eq.). The reaction was stirred at 20° C. for 6 h. The solvent was removed under reduced pressure and the crude was partitioned between water and EtOAc. The organic layer was discarded and the aqueous layer was neutralized by addition of aqueous HCl (2N) and thoroughly extracted with EtOAc. The organic layers were combined, dried over MgSO4, filtered and concentrated under reduced pressure to afford 1-[2-(3,5-dimethyl-phenyl)-acetyl]-2-methyl-azetidine-2-carboxylic acid.
後処理
- customThe solvent was removed under reduced pressure
- customthe crude was partitioned between water and EtOAc
- additionthe aqueous layer was neutralized by addition of aqueous HCl (2N)
- extractionthoroughly extracted with EtOAc
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-e2ffb32b6f0e4605973395909221a88f
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08759334B2
関連ノート
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