反応 #44693

反応方程式

compound

2-Amino-6-(4-pyridinyl)-4-pyrimidinol

phosphoryl chloride

N,N-dimethylaniline

→

4-Chloro-6-(4-pyridinyl)-2-pyrimidinamine

反応条件

後処理

1. 1
   workup.STIRRINGThe reaction solution is then stirred at room temperature for another two hours
2. 2
   その他The phosphoryl chloride is removed under reduced pressure
3. 3
   その他a rotary evaporator
4. 4
   workup.ADDITIONWater/dichloromethane 9:1 is added to the residue, which
5. 5
   workup.WAITis then boiled for 5 minutes
6. 6
   ろ過the product is filtered off with suction
7. 7
   その他dried under high vacuum

実験手順

32 g (170.04 mmol) of the compound (from example XXVIII) are dissolved in 87.1 ml (0.93 mmol) of phosphoryl chloride. 2.80 ml (22.11 mmol) of N,N-dimethylaniline are slowly added dropwise, and the mixture is stirred at 100° C. for one hour. The reaction solution is then stirred at room temperature for another two hours. The phosphoryl chloride is removed under reduced pressure using a rotary evaporator. Water/dichloromethane 9:1 is added to the residue, which is then boiled for 5 minutes. The mixture is then neutralized using saturated sodium bicarbonate solution and the product is filtered off with suction and dried under high vacuum.

出典