Hydrochloric Acid → HCID 178481777、化合物
反応式
[NH2:1][C:2]1[C:3](=[O:10])[N:4]([CH3:9])[N:5]=[CH:6][C:7]=1[NH2:8].Cl.[N:12]([O-])=O.[Na+]>O>[CH3:9][N:4]1[C:3](=[O:10])[C:2]2[N:1]=[N:12][NH:8][C:7]=2[CH:6]=[N:5]1参加物
5
実験手順
In water (10 ml) was dissolved 4,5-diamino-2-methyl-3(2H)-pyridazinone (280 mg) followed by addition of concentrated hydrochloric acid (0.5 ml) with ice-cooling. Then, sodium nitrite (290 mg)/water (5 ml) was added dropwise at a temperature not exceeding 10° C. and the mixture was stirred at that temperature for 1 hour and then at 100° C. for 1 hour. This reaction mixture was allowed to stand in the refrigerator for 16 hours and the resulting precipitate was collected by filtration, rinsed with water, and dried. White powder, 262 mg. 1H-NMR (DMSO-d6) δ: 3.76(3H,s), 8.71(1H,s).
後処理
- temperaturecooling
- customexceeding 10° C.
- waitat 100° C. for 1 hour
- waitto stand in the refrigerator for 16 hours
- filtrationthe resulting precipitate was collected by filtration
- washrinsed with water
- customdried
出典と根拠
- ORDレコード
- ord-97cc51c2622c46bda682c72f44df0dfb
- 出典データセット
- uspto-grants-1998_05
- 特許番号
- US05753664
反応ノート
読み込み中…