Sodium Hydroxide → 4-chloro-3-cyano-5-methyl-1H-pyrrole-2-carboxylic acid
反応式
[Cl:1][C:2]1[C:3]([C:13]#[N:14])=[C:4]([C:8]([O:10]CC)=[O:9])[NH:5][C:6]=1[CH3:7].[OH-].[Na+]>CO.O>[Cl:1][C:2]1[C:3]([C:13]#[N:14])=[C:4]([C:8]([OH:10])=[O:9])[NH:5][C:6]=1[CH3:7]参加物
5
実験手順
A solution of 670 mg (3.2 mmol) of ethyl 4-chloro-3-cyano-5-methyl-1H-pyrrole-2-carboxylate (Intermediate 193) and 3.2 ml (3.2 mmol) 1N NaOH in 20 ml MeOH was heated at 100° C. in a microwave reactor for 2 h. The mixture was diluted with water and extracted with EtOAc. The EtOAc was washed with 1N NaOH. The combined aqueous layers were acidified with concentrated HCl and extracted 2 times with EtOAc, each extract being washed with brine. Drying (MgSO4) and removal of solvent gave 535 mg of product as a solid. MS (ES) (M−H−): 183 for C7H5ClN2O2; NMR (d6-DMSO): 2.2 (s, 3H), 12.9 (s, 1H), 13.3 (s, 1H).
後処理
- extractionextracted with EtOAc
- washThe EtOAc was washed with 1N NaOH
- extractionextracted 2 times with EtOAc
- washeach extract being washed with brine
- customDrying
- custom(MgSO4) and removal of solvent
出典と根拠
- ORDレコード
- ord-d0cf9f87f81a4d89bf77774d8885c384
- 出典データセット
- uspto-grants-2013_03
- 特許番号
- US08399489B2
反応ノート
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