反応式
C(=O)([O-])[O-].[Na+].[Na+].[C:7]([CH2:10][NH:11][C:12]1[CH:20]=[CH:19][CH:18]=[CH:17][C:13]=1[C:14]([OH:16])=[O:15])([OH:9])=[O:8].[C:21](OC(=O)C)(=[O:23])[CH3:22].Cl>O>[C:21]([N:11]([CH2:10][C:7]([OH:9])=[O:8])[C:12]1[CH:20]=[CH:19][CH:18]=[CH:17][C:13]=1[C:14]([OH:16])=[O:15])(=[O:23])[CH3:22]参加物
6
実験手順
To a solution of sodium carbonate (89 g, 0.84 mol) in water (830 mL), 2-(carboxymethylamino)benzoic acid of Example 1a (100 g, 0.84 mol) was added in small portions at room temperature under stirring while a clear solution was formed. Acetic anhydride (85.68 g, 0.84 mol) was added dropwise at room temperature under stirring. The reaction mixture was stirred for 30 min, and 37% aqueous hydrochloric acid (140 mL) was added dropwise. The product precipitated slowly. The solid product was filtered off in 12 h, washed with water (3×150 mL) and air-dried to afford 110 g (91%), m.p. 206° C.
後処理
- customwas formed
- stirringunder stirring
- stirringThe reaction mixture was stirred for 30 min
- customThe product precipitated slowly
- filtrationThe solid product was filtered off in 12 h
- washwashed with water (3×150 mL)
- customair-dried
- customto afford 110 g (91%), m.p. 206° C.
出典と根拠
- ORDレコード
- ord-dfba3fce230f4807a8668f1996cd9fbf
- 出典データセット
- uspto-grants-2010_10
- 特許番号
- US07820691B2
関連ノート
読み込み中…