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CAS No. : | 93587-23-6 | MDL No. : | MFCD09999206 |
Formula : | C6H4BrN3O | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | HNQUXIMIIVPBPC-UHFFFAOYSA-N |
M.W : | 214.02 | Pubchem ID : | 135743711 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
97% | With N-Bromosuccinimide; In N,N-dimethyl-formamide; for 18.0h; | Intermediate 97 (1.70 g, 12.6 mmol) and NBS (2.69 g, 15.1 mmol) were dissolved in DMF (100 mL) and stirred for 18 h. The reaction mixture was diluted with water (50 mL) and the resulting solid was collected by filtration, dried, suspended in MeOH and filtered. The filtrate was concentrated in vacuo to give the title compound as a beige solid (2.60 g,97%). LCMS (ES+): 213.9, 215.9 (M+H)+. |
With N-Bromosuccinimide; In N,N-dimethyl-formamide; at 20℃; for 18.0h; | Example 49: l-(4-Chloro-5H-pyrrolo[3,2-rf]pyrimidin-7-yl)-2,2,2-trifluoro-l-[l-(4- fluorophenyl)-lH-indazol-5-yl]ethanol; A mixture of 3,5-dihydropyrrolo[3,2-T|pyrimidin-4-one (200 mg, 1.5 mmol, 1 equiv.) and N- bromosuccinimide (320 mg, 1.8 mmol, 1.2 equiv.) in 10 mL of DMF was stirred for 18 hours at room temperature. The reaction was diluted with water and resulting solid was collected by filtration, dried, suspended in MeOH, and filtered. The filtrate was concentrated in vacuo to provide 7-bromo-3,5-dihydropyrrolo[3,2-d]pyrimidin-4-one as a beige solid which was used without further purification. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
93% | A mixture of 7-bromo-3,5-dihydropyrrolo[3,2-?]pyrimidin-4-one (100 mg, 0.5 mmol) and 6 mL of POCI3 under argon was warmed at 115C. After 3 hours, the mixture was cooled to room temperature and poured over 300 mL of ice, stirred, made basic with potassium carbonate and extracted with EtOAc. The combined organic layers were dried, filtered, and concentrated in vacuo to provide 101 mg (93%) of the desired 7-bromo-4-chloro-5H-pyrrolo[3,2- djpyrimidine as beige solid which was used without further purification. | |
90% | With trichlorophosphate; for 2.0h;Inert atmosphere; Reflux; | Under argon atmosphere, a solution of 7-Bromo-3,5-dihydro-pyrrolo[3,2-d]pyrimidin-4-one (500 mg, 2.33 mmol) in phosphorus(V) oxychoride (6 rriL) was refluxed for 2 hours. The reaction mixture was then cooled to room temperature, concentrated and the residue was diluted with ethyl acetate. The organic layer was washed with a solution of sodium bicarbonate, brine, dried over sodium sulfate, filtered and evaporated under reduced pressure to afford compound (66a) as a pale solid (490 mg, 2.10 mmol, 90%) without further purification. lH NMR (400 MHz, DMSO-i delta 8.24 (d, J = 3.0 Hz, 1H), 8.72 (s, 1H), 12.95 (bs, 1H). MS m/z ([M+H]+) 232/234 |
35% | With trichlorophosphate; at 115℃; for 3.0h; | Intermediate 98 (1.30 g, 6.07 mmol) was suspended in POCI3 (60 mL) and heated at 115 C for 3 h. The reaction mixture was cooled to r.t. and poured cautiously onto ice (300 mL). The reaction mixture was basified with K2CO3 and extracted with EtOAc (3 x 200 mL). The combined organic fractions were dried (MgS04) and concentrated in vacuo to give the title compound as a beige solid (490 mg, 35%). LCMS (ES+): 231.9, 233.9, 235.9 (M+H)+. |
35% | With trichlorophosphate; at 115℃; for 3.0h; | Intermediate 98 (1.30 g, 6.07 mmol) was suspended in POCl3 (60 mL) and heated at 115 C. for 3 h. The reaction mixture was cooled to r.t. and poured cautiously onto ice (300 mL). The reaction mixture was basified with K2CO3 and extracted with EtOAc (3*200 mL). The combined organic fractions were dried (MgSO4) and concentrated in vacuo to give the title compound as a beige solid (490 mg, 35%). LCMS (ES+): 231.9, 233.9, 235.9 (M+H)+. |
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