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CAS No. : | 22536-61-4 | MDL No. : | MFCD09260903 |
Formula : | C5H5ClN2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | APRMCBSTMFKLEI-UHFFFAOYSA-N |
M.W : | 128.56 | Pubchem ID : | 581719 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H302 | Packing Group: | |
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 |
---|---|---|
92% | With ammonia; In ethanol; water; at 200℃; for 4h;Sealed tube; | Step 1 : To a solution of compound 184 (10.0 g, 77.79 mmol) in IMS (100 ml.) was added aqueous ammonia (35%, 100 ml). The reaction mixture was transferred to a sealed bomb and heated at 200 C for 4 h. The reaction mixture was allowed to cool to room temperature and was concentrated to remove most of the solvent and water (25 ml.) added. The solid obtained was filtered and dried under vacuum to give the desired compound 185 as off-white solid (7.85 g, 92% yield).1H NMR (400 MHz, DMSO-d6) delta 8.06 (s, 2H), 6.30 (s, 2H), 2.03 (s, 3H). LCMS m/z 1 10 [M+H]+. |
With ammonium hydroxide; at 85℃; for 18h;Sealed tube; | A mixture of 2-chloro-5-methylpyrimidine (1 g, 7.78 mmol) and ammonium hydroxide (18.26 mL, 469 mmol) was heated at 85 C in a sealed tube for 18 h. The mixture was cooled to rt and and then ice/water bath, and filtered. The white filter cake was washed with hexanes and suction dried.LCMS (method C ) tR,0.33 min., MH+ = 110.2 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1.62 g | With potassium phosphate; tris-(dibenzylideneacetone)dipalladium(0); tricyclohexylphosphine; In 1,4-dioxane; water; at 100℃; for 24h;Inert atmosphere; | [01332j 2-(3,4-Dihydro-2H-pyran-6-yl)-5-methylpyrimidine, Example643.1. A mixture of 2-chloro-5-methylpyrimidine (1.2 g, 9.33 mmol), 3,4-dihydro-2h- pyran-6-boronic acid pinacol ester (2.94 mL, 14.0 mmol), tricyclohexyiphosphine (0.524 g, 1.87 mmol) and tris-(dibenzylideneacetone) dipalladium (0) (0.855 g, 0.93 mmol) inflask was degassed and backfilled with argon. To this mixture were added 1,4-dioxane (16 mL) and potassium phosphate tribasic (6.45 g, 28.0 mmol) in water (2.0 mL). A stream of argon was bubbled through the resulting mixture for an additional 5 minutes, and the mixture was stirred at 100 C under a balloon of argon for 24 hours. The mixture was cooled to RT, filtered, and washed with EtOAc. The filtrate was concentrated in vacuo, and the residue was purified by Isco CombiFlash on a RediSep 80 g silica gel column using 0-100% EtOAc gradient in heptane as the eluent to give Example 643.1 (1.62 g). ?H NMR (400 MI-Tz, CDC13) 8.48 (s, 2H), 6.26 (t, J= 4.1, 4.1 Hz, 1H), 4.21- 4.24 (m, 2H), 2.20-2.26 (obscured m, 2H), 2.25 (s, 3H), 1.9 (dd, J= 5.6, 4.8 Hz, 2H). LCMS (pos.)m/z: 177.1 (M+H). |
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