Reaktion #60768

Reaktionsgleichung

4-Amino-3-(4-aminophenyl)thieno[2,3-d]pyrimidine

isocyanate

2-fluoro-5-trifluoromethyl-phenyl isocyanate

diisopropylethylamine

→

4-Amino-3-(4-((2-fluoro-5-(trifluoromethyl)phenyl)-aminocarbonylamino)phenyl)thieno[2,3-d]pyrimidine

Lösungsmittel

methanol triethylamine

—

amine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenconcentrated to dryness in a Speedvac system
2. 2
   Sonstigepurified by prep HPLC
3. 3
   workup.ADDITIONThe fraction containing the desired product
4. 4
   Sonstigewas collected
5. 5
   Einengenconcentrated to dryness

Vorschrift

4-Amino-3-(4-aminophenyl)thieno[2,3-d]pyrimidine (0.2 mmoles) was dissolved in 1 mL amine-free DMF and treated with 0.3 mmoles of the isocyanate of choice (2-fluoro-5-trifluoromethyl-phenyl isocyanate) and 0.6 mmoles of diisopropylethylamine for 2 hours at room temperature. The reaction mixture was treated with 0.5 mL 1:1 methanol-triethylamine for half an hour and concentrated to dryness in a Speedvac system, reconstituted in 1 mL DMSO and purified by prep HPLC. The fraction containing the desired product was collected and concentrated to dryness. MH+=448.

Quelle