反応 #3541

反応方程式

2,7-diamino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidine

sulfamic acid

diethylaminoethylamine

→

6-(2,6-dichlorophenyl)-N2 -(2-diethylamino-ethyl)-pyrido[2,3-d]pyrimidine-2,7-diamine

NH3

収率 1.0%

反応条件

後処理

1. 1
   その他The excess diethylaminoethylamine was removed in vacuo
2. 2
   workup.DISSOLUTIONThe resulting oil was dissolved in diethyl ether
3. 3
   workup.ADDITIONdiluted with hexane
4. 4
   ろ過filtered
5. 5
   workup.DISSOLUTIONThe resulting solid was dissolved in dichloromethane which
6. 6
   洗浄was washed several times with water
7. 7
   乾燥dried with magnesium sulfate
8. 8
   濃縮concentrated in vacuo
9. 9
   その他The residue was crystallized from ethyl acetate

実験手順

A mixture of 2,7-diamino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidine (4.0 g) from Example 1, sulfamic acid (2.53 g), and diethylaminoethylamine (40 mL) was heated to approximately 150° C. for 20 hours. The excess diethylaminoethylamine was removed in vacuo. The resulting oil was dissolved in diethyl ether, diluted with hexane, and then filtered. The resulting solid was dissolved in dichloromethane which was washed several times with water, dried with magnesium sulfate, and concentrated in vacuo. The residue was crystallized from ethyl acetate to give the title compound 6-(2,6-dichlorophenyl)-N2 -(2-diethylamino-ethyl)-pyrido[2,3-d]pyrimidine-2,7-diamine, CIMS (1% NH3 in CH4): 433=M+ +C2H5, 405=M+ +H, 389=M+ -Et, 360; mp 216°-219.5° C.

出典