반응 #55080
ord-80bb9ca87dee465e97accc18056e570b
반응 방정식
반응 조건
후처리
- 1온도The mixture is heated
- 2온도under reflux for 4 hours
- 3세척washed with water and with dilute bicarbonate solution
- 4기타dried
- 5기타The mixture is evaporated in vacuo
- 6기타After leaving the reactants in contact overnight
- 7기타the mixture is evaporated to dryness in vacuo
- 8여과the mixture is filtered over charcoal
- 9기타the filtrate is precipitated with 3 N HCl
- 10추출the product is extracted with ether
- 11기타the extract is dried
- 12기타evaporated
- 13기타the product is crystallised in diisopropyl ether
실험 절차
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.