Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List 2,4-dichloro-5,7-dihydrothieno[3,4-d]pyriMidine

2,4-dichloro-5,7-dihydrothieno[3,4-d]pyriMidine synthesis

5synthesis methods
-

Yield:74901-71-6 1.6 g

Reaction Conditions:

with P,P-dichlorophenylphosphine oxide at 135 - 165;

Steps:

1; 1.v

Step (v)To thieno[3,4-d]pyrimidine-2,4-(lH, 3H, 5H, 7H)-dione (1.6 g, 9.41 mmol) was suspended in 4.0 mL of phenylphosphonyl dichloride and the suspension heated overnight at 135 °C, then for 1 hour at 165 °C. The resulting reaction mixture was cooled down and poured into ice-water. The aqueous layer was extracted with ethyl acetate. The organic layers were combined, washed with saturated NaHC03 solution and brine, dried over anhydrous Na2S04 and evaporated. The crude product was then purified by column chromatography on silica gel (eluent: PE/EA=20/1-10/1) to give 2,4-dichloro-5,7-dihydrothieno[3,4-d]pyrimidine as a light yellow solid(l .6 g, 83%).LC-MS (Method A), (ES+)207/ 209, RT = 4.96 min.

References:

WO2013/50508,2013,A1 Location in patent:Page/Page column 42; 56