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ChemicalBook CAS DataBase List 5-Chloro-3-iodopyrazolo[1,5-a]pyrimidine
923595-58-8

5-Chloro-3-iodopyrazolo[1,5-a]pyrimidine synthesis

2synthesis methods
-

Yield:923595-58-8 100%

Reaction Conditions:

with N-iodo-succinimide in N,N-dimethyl-formamide at 20;

Steps:

1.5 5-chloro-3-iodopyrazolo[1,5-a]pyrimidine

To a solution of 5-chloropyrazolo[1,5-a]pyrimidine (200 mg, 1.30 mmol) in DMF (2 mL) was added N-iodosuccinimide (322 mg, 1.86 mmol). The reaction was stirred at rt overnight, then diluted with EtOAc (100 mL), and washed with H2O (50 mL), saturated Na2S2O3 aqueous solution (50 mL) and brine (50 mL). The separated organic phase was dried over anhydrous Na2SO4, and concentrated in vacuo. The residue was purified by a silica gel column chromatography (EtOAc/PE (v/v)=1/4) to give the title compound as a pale yellow solid (390 mg, 100%). [0309] MS (ESI, pos. ion) m/z: 279.9 [M+H]+. [0310] 1H NMR (400 MHz, CDCl3) δ (ppm): 8.57 (d, J=7.2 Hz, 1H), 8.16 (s, 1H), 6.86 (d, J=7.2 Hz, 1H)

References:

US2014/234254,2014,A1 Location in patent:Paragraph 0308; 0309; 0310

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