تفاعل #56459
ord-abd2d97cd76d49eabf871b9bb464d08c
معادلة التفاعل
الكواشف
ظروف التفاعل
المعالجة
- 1درجة الحرارةThe mixture is heated to 50°-60° C.
- 2درجة الحرارةThe mixture is heated
- 3درجة الحرارةunder reflux
- 4درجة الحرارةboiling is maintained for 15 minutes
- 5درجة الحرارةThe mixture is cooled
- 6درجة الحرارةThe mixture is again heated
- 7درجة الحرارةunder reflux for 30 minutes
- 8درجة الحرارةcooled
- 9أخرىat 60°-70° C
- 10درجة الحرارةThe whole is then heated
- 11درجة الحرارةunder reflux for 30 minutes
- 12درجة الحرارةcooled
- 13ترشيحfiltered
- 14أخرىthe precipitate obtained
- 15ترشيحis filtered off the redissolved cold in dilute sodium bicarbonate solution
- 16غسيلthis solution is washed with methylene chloride
- 17ترشيحfiltered
الإجراء التجريبي
15.2 g (0.2 mol) of thiourea in 100 ml of water are introduced into a 1 liter 3-necked flask. The mixture is heated to 50°-60° C. and 39.1 g (0.2 mol) of 2,4-dichlorobenzylchloride are introduced in a single operation. The mixture is heated under reflux and boiling is maintained for 15 minutes; the solution becomes limpid. The mixture is cooled and a solution of 32 g (0.8 mol) of NaOH in 50 ml of water is introduced dropwise at about 60° C. The mixture is again heated under reflux for 30 minutes, cooled and a solution of about 0.28 mol of sodium chloroacetate (obtained by neutralising 26.46 g of chloroacetic acid in 200 ml of water with 23.52 g of NaHCO3) is introduced, dropwise, at 60°-70° C. The whole is then heated under reflux for 30 minutes, cooled, filtered and acidified with 3 N HCl; the precipitate obtained is filtered off the redissolved cold in dilute sodium bicarbonate solution, and this solution is washed with methylene chloride, filtered and again acidified. 41.7 g (yield: 83 %) of product are thus collected. Instantaneous melting point: 72°-73° C.