反応 #51441

反応方程式

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

溶媒

acetic acid

反応条件

後処理

1. 1
   温度The mixture is refluxed for 4 hours
2. 2
   ろ過the mixture is then filtered
3. 3
   洗浄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
   その他the solid precipitated
6. 6
   ろ過is filtered off
7. 7
   洗浄This is washed twice with 500 ml of water
8. 8
   ろ過filtered off
9. 9
   その他dried in vacuo at 45° C

実験手順

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%)

出典