反応 #807663

反応方程式

5-Chloro-2-methylphenyl isothiocyanate

methylamine hydrochloride

Triethylamine

→

N-(5-chloro-2-methylphenyl)-N′-methylthiourea

収率 96.9%

溶媒

chloroform

反応条件

後処理

1. 1
   workup.STIRRINGThe mixture was stirred for 18 hours
2. 2
   その他The solvent was evaporated
3. 3
   workup.ADDITIONThe residue was treated with ethyl acetate (800 mL) and water (400 mL)
4. 4
   その他The organic phase was separated
5. 5
   洗浄washed with water (2×300 mL)
6. 6
   乾燥dried over magnesium sulfate
7. 7
   その他evaporated to dryness

実験手順

5-Chloro-2-methylphenyl isothiocyanate (36.6 g; 0.2 mol) was added to the solution of methylamine hydrochloride (26.8 g; 0.4 mol) in chloroform (300 mL). Triethylamine (65 mL; 0.47 mol) was added dropwise while stirring at ambient temperature. The mixture was stirred for 18 hours. The solvent was evaporated. The residue was treated with ethyl acetate (800 mL) and water (400 mL). The organic phase was separated, washed with water (2×300 mL), dried over magnesium sulfate and evaporated to dryness to give 41.6 g of N-(5-chloro-2-methylphenyl)-N′-methylthiourea, m.p. 139–140° C.

出典