反応式
[CH3:1][NH:2][C:3](=[O:6])[CH2:4][NH2:5].F[C:8]1[C:25](F)=[CH:24][C:23]([I:27])=[CH:22][C:9]=1[C:10]([C:12](=[CH:18]OCC)[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[O:11].[H-].[Na+]>CN1C(=O)CCC1>[I:27][C:23]1[CH:22]=[C:9]2[C:10](=[O:11])[C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:18][N:5]3[CH2:4][C:3](=[O:6])[N:2]([CH3:1])[C:25]([CH:24]=1)=[C:8]23参加物
5
反応条件
- 温度
- 100 °C
実験手順
Glycine methylamide (1.0 g) is added at room temperature to a solution of ethyl 2-(2,3-difluoro-5-iodobenzoyl)-3-ethoxy-2-propenoate (Preparation 21, 2.0 g) in NMP (20 mL). Sodium hydride (400 mg, 60% dispersion in mineral oil) is added in two portions to the solution, and the solution is heated at 100° C. for 30 min. The product is partitioned between chloroform and water, the chloroform phase is concentrated and applied to a silica gel column with 1-2% methanol chloroform as the eluant. The purified fractions are triturated with ether to give 1.22 g of the title compound. Physical characteristics: M.p. 278-283° C.; 1H NMR (DMSO-d6) δ1.29, 3.63, 4.23, 5.10, 7.65, 8.09, 8.55. Anal. Found: C, 43.49; H, 3.18; N, 6.75.
後処理
- customThe product is partitioned between chloroform and water
- concentrationthe chloroform phase is concentrated
- customThe purified fractions are triturated with ether
出典と根拠
- ORDレコード
- ord-716885f811cd43c5882c170472049ab2
- 出典データセット
- uspto-grants-2003_09
- 特許番号
- US06624159B2
関連ノート
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