反応 #54722

反応方程式

2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide

methylene chloride

chloroformic acid octyl ester

→

dioctyl 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide

溶媒

triethylamine

反応条件

後処理

1. 1
   温度The mixture is cooled for 30 minutes
2. 2
   workup.STIRRINGstirred at room temperature for 1 hour
3. 3
   抽出The mixture is extracted with methylene chloride
4. 4
   洗浄washed with water
5. 5
   乾燥dried over magnesium sulfate
6. 6
   その他evaporated under reduced pressure
7. 7
   その他The residue is recrystallized from methylene chloride/ethanol, there

実験手順

10 G. of 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide are suspended in 150 ml. of methylene chloride and 20 ml. of triethylamine. The suspension is cooled to 5° C. and 28 g. of chloroformic acid octyl ester are added dropwise while stirring. The mixture is cooled for 30 minutes and then stirred at room temperature for 1 hour. The mixture is extracted with methylene chloride, washed with water, dried over magnesium sulfate and evaporated under reduced pressure. The residue is recrystallized from methylene chloride/ethanol, there being obtained dioctyl 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 64° C.

出典