تفاعل #55080

معادلة التفاعل

hydroxylamine

sodium methylate

3,4-dichlorobenzylthioacetic acid

H2SO4

dichloroethane

→

stated product

المردود 75.0%

3,4-Dichlorobenzylthioaceto-hydroxamic acid

المردود 75.0%

المذيبات

methanol

methanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture is heated
2. 2
   درجة الحرارةunder reflux for 4 hours
3. 3
   غسيلwashed with water and with dilute bicarbonate solution
4. 4
   أخرىdried
5. 5
   أخرىThe mixture is evaporated in vacuo
6. 6
   أخرىAfter leaving the reactants in contact overnight
7. 7
   أخرىthe mixture is evaporated to dryness in vacuo
8. 8
   ترشيحthe mixture is filtered over charcoal
9. 9
   أخرىthe filtrate is precipitated with 3 N HCl
10. 10
    استخلاصthe product is extracted with ether
11. 11
    أخرىthe extract is dried
12. 12
    أخرىevaporated
13. 13
    أخرىthe product is crystallised in diisopropyl ether

الإجراء التجريبي

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.

المصدر