反应 #51441

反应方程式

charcoal

hydriodic acid

( 6 )

[6-(4-amino-4-methylpiperidin-1-yl)-2-chloro-7,8-dihydropyrimido[5,4-d]pyrimidin-4-yl]-(3-chloro-4-fluorophenyl)amine

→

6-(4-amino-4-methylpiperidin-1-yl)-4-(3-chloro-4-fluorophenylamino)-pyrimido[5,4-d]pyrimidine

溶剂

acetic acid

反应条件

后处理

1. 1
   温度The mixture is refluxed for 4 hours
2. 2
   过滤the mixture is then filtered
3. 3
   洗涤the residue is washed with glacial acetic acid and water
4. 4
   workup.ADDITIONThe filtrate is added dropwise, with vigorous stirring, to a solution of 270 ml water, 270 ml of methanol and 270 ml of sodium hydroxide solution (50%)
5. 5
   其他the solid precipitated
6. 6
   过滤is filtered off
7. 7
   洗涤This is washed twice with 500 ml of water
8. 8
   过滤filtered off
9. 9
   其他dried in vacuo at 45° C

实验过程

A mixture of 80 g (0.182 mol) of (6) in 160 ml glacial acetic acid at 90° C. is added dropwise to a suspension of 11.7 g (0.378 mol) of red phosphorus in 150 ml of hydriodic acid (57%, 1.134 mol). The mixture is refluxed for 4 hours, 5 g of activated charcoal are added, the mixture is then filtered and the residue is washed with glacial acetic acid and water. The filtrate is added dropwise, with vigorous stirring, to a solution of 270 ml water, 270 ml of methanol and 270 ml of sodium hydroxide solution (50%). The mixture is stirred for a further 30 minutes at 15° C. and the solid precipitated is filtered off. This is washed twice with 500 ml of water, then suspended in 500 ml of water, filtered off and dried in vacuo at 45° C. Yield: 65.2 g (91.9%)

来源