反応式
P(Cl)(Cl)(Cl)(Cl)[Cl:2].[N:7]([C:9]1[CH:18]=[CH:17][C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]=1[OH:19])=O>CCCCCC>[Cl:2][C:10]([C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:16]=1/[CH:17]=[CH:18]\[C:9]#[N:7])=[O:19]参加物
実験手順
To a rapidly stirring suspension of phosphorus pentachloride (197.5 g) in dry hexane (3.5 liters) is added 167.0 g (0.964 mole) of 2-nitroso-1-naphthol. The mixture is stirred at room temperature for 1 hour after which it is refluxed for 1 hour, cooled slightly and decanted while hot. The residue is boiled with hexane (3.0 liters) for another hour after which the solution is decanted and combined with the first hexane extract. It is evaporated down to dryness. Yield: 200.0 g (crude). This residue is extracted with hexane (2.0 liters), the hexane decanted, cooled, and the resultant crystals are filtered off. The filtrate is used to reestract additional compound from the above residue (the reextraction being repeated four times) with cooling and filtering of the crystals obtained each time. Yield: 79.0 g (42.5%), mp=72°-74°.
後処理
- stirringThe mixture is stirred at room temperature for 1 hour after which it
- temperatureis refluxed for 1 hour
- temperaturecooled slightly
- customdecanted while hot
- waitThe residue is boiled with hexane (3.0 liters) for another hour
- customafter which the solution is decanted
- extractionextract
- customIt is evaporated down to dryness
- extractionThis residue is extracted with hexane (2.0 liters)
- customthe hexane decanted
- temperaturecooled
- filtrationthe resultant crystals are filtered off
- temperaturewith cooling
- filtrationfiltering of the crystals
- customobtained each time
出典と根拠
- ORDレコード
- ord-2ccce5b6b95b432bacc83489aeb5669d
- 出典データセット
- uspto-grants-1976_10
- 特許番号
- US03985731
関連ノート
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