Hydroxyamine hydrochloride → HCID 135980741, 화합물
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[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]참가 물질
5
실험 절차
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%.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-791ea7c176f44afc951865db679f5e53
- 출처 데이터셋
- uspto-grants-1998_06
- 특허 번호
- US05773624
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