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ChemicalBook CAS DataBase List 2,4,6-trichloro-pyrido[2,3-d]pyrimidine
958360-30-0

2,4,6-trichloro-pyrido[2,3-d]pyrimidine synthesis

6synthesis methods
Pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione, 6-chloro-

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2,4,6-trichloro-pyrido[2,3-d]pyrimidine

958360-30-0
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Yield:958360-30-0 88%

Reaction Conditions:

with P,P-dichlorophenylphosphine oxide at 180; for 6 h;

Steps:

42.b Synthesis of 2,4,6-trichloropyrido[2,3-d]pyrimidine

The mixture of 6-chloropyrido[2,3-d]pyrimidin-2,4(1H,3H)-dione (163.0 mg, 0.82 mmol) and BPOD (2.0 mL) was stirred at 180° C. for 6 hours and then cooled to room temperature. The reaction mixture was poured into water, and it was neutralized with saturated NaHCO3 aqueous solution (pH=7) and then extracted with EtOAc (30.0 mL). The organic layer was washed with brine, dried over anhydrous Na2SO4, filtered and then distilled under reduced pressure to obtain white solid compound of 2,4,6-trichloropyrido[2,3-d]pyrimidine (169.0 mg, 88%). [0694] 1H-NMR (300 MHz, DMSO-d6); δ: 8.97 (d, 1H, J=2.8 Hz), 8.49 (d, 1H, J=2.8 Hz)

References:

US2014/315888,2014,A1 Location in patent:Paragraph 0693-0694

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