反応 #42624

反応方程式

4-chloro-2-isopropyl-6-methylpyrimidine

dodecylamine

ethyl acetate

sodium hydroxide

→

4-dodecylamino-2-isopropyl-6-methylpyrimidine

溶媒

dioxane

dioxane

反応条件

後処理

1. 1
   温度After cooling
2. 2
   洗浄the organic phase is washed with 300 ml of water, and 10 ml of saturated NaCl solution
3. 3
   workup.ADDITIONare added
4. 4
   その他The organic phase is separated off
5. 5
   濃縮concentrated
6. 6
   workup.DISTILLATIONthe excess dodecylamine is distilled in vacuo up to a bath temperature of 160° C

実験手順

79.2 g of 4-chloro-2-isopropyl-6-methylpyrimidine (464.1 mmol) are heated in 100 ml of dioxane at 100° C. A heated solution of 189.3 g of dodecylamine (1021 mmol, 2.2 eq) in 30 ml of dioxane is added dropwise thereto over the course of 2 hours, and the reaction mixture is further heated for 2 hours at 100° C. and for 9 hours at 109° C. After cooling, 400 ml of ethyl acetate and 150 ml of 4M sodium hydroxide solution (600 mmol) are added thereto and the mixture is stirred at 50° C. for 10 minutes. The lower, aqueous phase is discarded, the organic phase is washed with 300 ml of water, and 10 ml of saturated NaCl solution are added thereto. The organic phase is separated off and concentrated, and the excess dodecylamine is distilled in vacuo up to a bath temperature of 160° C. 136.1 g (91.8%); GC purity: 98%

出典