Reaktion #3541

Reaktionsgleichung

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

Ausbeute 1.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe 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
   Filtrationfiltered
5. 5
   workup.DISSOLUTIONThe resulting solid was dissolved in dichloromethane which
6. 6
   Waschenwas washed several times with water
7. 7
   Trocknendried with magnesium sulfate
8. 8
   Einengenconcentrated in vacuo
9. 9
   SonstigeThe residue was crystallized from ethyl acetate

Vorschrift

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.

Quelle