Hydroxyamine hydrochloride → HCID 135980741、化合物
反応式
[C:1]([C:3](=[N:7][O:8][CH3:9])[C:4](N)=[O:5])#[N:2].C(=O)(O)[O-:11].[Na+].Cl.[NH2:16][OH:17]>O>[C:4]([C:3](=[N:7][O:8][CH3:9])[C:1](=[N:16][OH:17])[NH2:2])([OH:11])=[O:5]参加物
5
実験手順
To a suspension of 2-cyano-2-methoxyimino-acetamide (24.4 g, 0.19 mol) and sodium bicarbonate (32.2 g, 0.38 mol) in water, hydroxylamine hydrochloride (13.3 g, 0.19 mol) in water (18.4 g) was added dropwise at 80° to 85° C. The mixture was stirred at the same temperature for 3 hrs. Then, the reaction solution was concentrated followed by adjusting to pH 2.0 with concentrated hydrochloric acid and then cooling to separate crystals. The crystals were filtered off, washed with methanol (20 g) and dried to give 2-carboxy-2-methoxyimino-acetamidoxime (27.1 g). The crystal contained 14.8% of sodium chloride. Practical yield: 27.1×0.852=23.1 g. Yield: 74.8%.
後処理
- additionwas added dropwise at 80° to 85° C
- concentrationThen, the reaction solution was concentrated
- temperaturecooling
- customto separate crystals
- filtrationThe crystals were filtered off
- washwashed with methanol (20 g)
- customdried
出典と根拠
- ORDレコード
- ord-791ea7c176f44afc951865db679f5e53
- 出典データセット
- uspto-grants-1998_06
- 特許番号
- US05773624
反応ノート
読み込み中…