Methane → HCID 21396807、化合物
反応式
[NH2:1][C:2]([O:9][CH2:10][CH2:11][CH3:12])=[C:3]([C:7]#[N:8])[C:4](=[S:6])[NH2:5].OO.C>C(O)C>[NH2:5][C:4]1[S:6][N:1]=[C:2]([O:9][CH2:10][CH2:11][CH3:12])[C:3]=1[C:7]#[N:8]参加物
5
実験手順
A mixture of 111 g of 3-amino-2-cyano-3-propoxypropene-thioamide in 250 ml of ethanol was heated to reflux. To this stirred mixture was added 20.4 g of 30% hydrogen peroxide, at such a rate as to maintain a uniform rate of reflux. After complete addition, the reaction mixture was heated under reflux for 20 minutes. A quantity of activated charcoal was added to the reaction mixture. The reaction mixture was filtered hot and allowed to cool. The filtrate was poured into 1500 ml of water, and the solid precipitate was collected by filtration. The dried solid was recrystallized from toluene, to give 104.5 g of 5-amino-4-cyano-3-propoxyisothiazole, m.p. 122°-125°.
後処理
- temperaturewas heated to reflux
- temperatureat such a rate as to maintain a uniform rate
- temperatureof reflux
- additionAfter complete addition
- temperaturethe reaction mixture was heated
- temperatureunder reflux for 20 minutes
- filtrationThe reaction mixture was filtered hot
- temperatureto cool
- additionThe filtrate was poured into 1500 ml of water
- filtrationthe solid precipitate was collected by filtration
- customThe dried solid was recrystallized from toluene
出典と根拠
- ORDレコード
- ord-45ae10aa13c442d1978445655465de9c
- 出典データセット
- uspto-grants-1977_11
- 特許番号
- US04059433
反応ノート
読み込み中…