反応式
[NH2:1][C:2]1[CH:10]=[C:9]([O:11][CH3:12])[CH:8]=[CH:7][C:3]=1[C:4](N)=[O:5].Cl.[OH-:14].[Na+]>>[NH2:1][C:2]1[CH:10]=[C:9]([O:11][CH3:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:14])=[O:5]参加物
4
実験手順
A solution of 27.4 g (0.165 mol) of 2-amino-4-methoxybenzamide in 500 mL of 1N sodium hydroxide was stirred and heated under reflux for 18 hours. After the reaction mixture had cooled to room temperature the solution was brought to pH 6-7 with 0.5N HCl. A white precipitate formed which was collected by vacuum filtration. The crystals were rinsed with water and dried overnight at 100° C. The product amounted to 23.9 g. An analytical sample (mp 176-178° C.) was obtained by recrystallization from ethyl acetate.
後処理
- temperatureheated
- temperatureunder reflux for 18 hours
- customA white precipitate formed which
- filtrationwas collected by vacuum filtration
- washThe crystals were rinsed with water
- customdried overnight at 100° C
- customAn analytical sample (mp 176-178° C.) was obtained by recrystallization from ethyl acetate
出典と根拠
- ORDレコード
- ord-675984d37fee4c66b5d8a3c04ab04ac6
- 出典データセット
- uspto-grants-1999_09
- 特許番号
- US05948775
関連ノート
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