反応 #807668

反応方程式

5-Chloro-2-methylphenyl isothiocyanate

2-propynylamine hydrochloride

triethyl amine

→

N-(5-chloro-2-methylphenyl)-N′-(2-propynyl)thiourea

収率 70.4%

溶媒

methylene chloride

反応条件

後処理

1. 1
   その他The mixture was evaporated to dryness
2. 2
   workup.STIRRINGThe residue was stirred in water (200 mL) for 1 hour
3. 3
   ろ過then filtered
4. 4
   workup.DISSOLUTIONThe solid was dissolved in ethyl acetate (300 mL)
5. 5
   洗浄washed with 1N hydrochloric acid (2×200 mL)
6. 6
   乾燥The organic phase was dried over anhydrous magnesium sulfate
7. 7
   その他evaporated to dryness

実験手順

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.

出典