反応 #3300

反応方程式

6-(2,6-dichlorophenyl)-8-ethyl-2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one

6-(2,6-Dichlorophenyl)-8-ethyl-2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one

4-methoxyaniline

→

6-(2,6-Dichlorophenyl)-8-ethyl-2-(4-methoxyphenylamino)-8H-pyrido[2,3-d]pyrimidin-7-one

溶媒

dimethylformamide

反応条件

後処理

1. 1
   温度at reflux for 10 minutes
2. 2
   その他Crystals separated on inducement
3. 3
   workup.ADDITIONAn additional 3 drops of water were added
4. 4
   その他to precipitate additional tacky solid
5. 5
   その他After decantation, the solid was triturated with 0.5 mL of ethyl acetate and 0.5 mL of petroleum ether
6. 6
   ろ過The solids were filtered
7. 7
   洗浄washed with 50% ethyl acetate/petroleum ether
8. 8
   その他dried
9. 9
   その他Purification
10. 10
    ろ過by filtering an ethyl acetate solution through a layer of silica gel
11. 11
    その他Concentration of the filtrate to 1 mL volume yielded pure crystalline product

実験手順

A solution of 0.100 g (0.25 mmol) of 6-(2,6-dichlorophenyl)-8-ethyl-2-methanesulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 68 and 0.061 g (0.50 mmol) of 4-methoxyaniline in 0.5 mL of dimethylformamide was heated at reflux for 10 minutes. Three drops of water were added. Crystals separated on inducement. An additional 3 drops of water were added to precipitate additional tacky solid. After decantation, the solid was triturated with 0.5 mL of ethyl acetate and 0.5 mL of petroleum ether. The solids were filtered and washed with 50% ethyl acetate/petroleum ether and dried; wt 0.080 g. Purification was effected by filtering an ethyl acetate solution through a layer of silica gel. Concentration of the filtrate to 1 mL volume yielded pure crystalline product; wt 0.033 g; mp 213°-215° C.

出典