반응 #56459
ord-abd2d97cd76d49eabf871b9bb464d08c
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반응 조건
후처리
- 1온도The mixture is heated to 50°-60° C.
- 2온도The mixture is heated
- 3온도under reflux
- 4온도boiling is maintained for 15 minutes
- 5온도The mixture is cooled
- 6온도The mixture is again heated
- 7온도under reflux for 30 minutes
- 8온도cooled
- 9기타at 60°-70° C
- 10온도The whole is then heated
- 11온도under reflux for 30 minutes
- 12온도cooled
- 13여과filtered
- 14기타the precipitate obtained
- 15여과is filtered off the redissolved cold in dilute sodium bicarbonate solution
- 16세척this solution is washed with methylene chloride
- 17여과filtered
실험 절차
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.