反応 #55080
ord-80bb9ca87dee465e97accc18056e570b
反応方程式
反応条件
後処理
- 1温度The mixture is heated
- 2温度under reflux for 4 hours
- 3洗浄washed with water and with dilute bicarbonate solution
- 4その他dried
- 5その他The mixture is evaporated in vacuo
- 6その他After leaving the reactants in contact overnight
- 7その他the mixture is evaporated to dryness in vacuo
- 8ろ過the mixture is filtered over charcoal
- 9その他the filtrate is precipitated with 3 N HCl
- 10抽出the product is extracted with ether
- 11その他the extract is dried
- 12その他evaporated
- 13その他the product is crystallised in diisopropyl ether
実験手順
20.2 g (0.08 mol) of 3,4-dichlorobenzylthioacetic acid are esterified with 10 ml of methanol, 0.6 ml of concentrated H2SO4 and 100 ml of dichloroethane. The mixture is heated under reflux for 4 hours, washed with water and with dilute bicarbonate solution, and dried. The mixture is evaporated in vacuo. The oily residue, in methanol, is treated with a solution of hydroxylamine (0.1 mol) in the presence of 0.18 mol of sodium methylate. After leaving the reactants in contact overnight, the mixture is evaporated to dryness in vacuo, the residue is taken up in water, the mixture is filtered over charcoal and the filtrate is precipitated with 3 N HCl, the product is extracted with ether, the extract is dried and evaporated and the product is crystallised in diisopropyl ether. 15 g of the stated product are obtained (yield 71%). Melting point: 75°-76° C.