反应详情

5-Chloro-2-methylphenyl isothiocyanate (18.3 g; 0.1 mol) was added dropwise to the mixture of 2-propynylamine hydrochloride (9.2 g, 0.1 mol) and triethyl amine (20 mL) in methylene chloride (200 mL). The mixture was stirred for 18 hours at ambient temperature. The mixture was evaporated to dryness. The residue was stirred in water (200 mL) for 1 hour then filtered. The solid was dissolved in ethyl acetate (300 mL) and washed with 1N hydrochloric acid (2×200 mL) then with water (300 mL). The organic phase was dried over anhydrous magnesium sulfate and evaporated to dryness to give 16.8 g of N-(5-chloro-2-methylphenyl)-N′-(2-propynyl)thiourea.

1. customThe mixture was evaporated to dryness
2. stirringThe residue was stirred in water (200 mL) for 1 hour
3. filtrationthen filtered
4. dissolutionThe solid was dissolved in ethyl acetate (300 mL)
5. washwashed with 1N hydrochloric acid (2×200 mL)
6. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
7. customevaporated to dryness