Acetic Anhydride → HCID 178526759、化合物
反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([NH:11][CH:12]=[CH:13][N+:14]([O-:16])=[O:15])=[C:6]([CH:10]=1)[C:7](O)=[O:8].C([O-])(=O)C.[K+].C(OC(=O)C)(=O)C>>[Br:1][C:2]1[CH:10]=[C:6]2[C:5](=[CH:4][CH:3]=1)[N:11]=[CH:12][C:13]([N+:14]([O-:16])=[O:15])=[C:7]2[OH:8]参加物
4
実験手順
29 g (101 mmol) of 5-bromo-2-(2-nitro-vinylamino)-benzoic acid (Example 1a) and 11.9 g (121 mmol) of potassium acetate in 129 ml (152 mmol) of acetic anhydride are stirred for 1.5 h at 120° C. The precipitate is filtered off and washed with acetic acid until the filtrate is colorless, then is washed with H2O and dried in vacuo to give the title compound. ES-MS: 269, 271 (M+H)+, Br pattern; analytical HPLC: W=2.70 min (Grad 1).
後処理
- filtrationThe precipitate is filtered off
- washwashed with acetic acid until the filtrate
- washis washed with H2O
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-1187ae13cd6e46169620e1450218914c
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09358229B2
反応ノート
読み込み中…