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CAS No. : | 957187-27-8 | MDL No. : | MFCD12828062 |
Formula : | C7H4BrClN2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | LMPPBTNPACXNDI-UHFFFAOYSA-N |
M.W : | 231.48 | Pubchem ID : | 26370038 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-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 |
---|---|---|
89% | In ethanol; water; at 50.0℃; | A mixture of 3-bromo-5-chloropyridin-2-amine (10 g, 49 mmol) and chloroacetaldehyde (50% in H2O, 12 mL, 98 mmol) in ethanol (100 mL) was heated at 50 C. overnight. It was then cooled to room temperature and concentrated. Acetone (30 mL) was added to the residue and the resulting mixture was stirred rapidly for 2 h. The resulting solid was collected through filtration and dried to afford 101a as a yellow solid (10.0 g, 89%). MS: [M+H]+231. 1H NMR (500 MHz, DMSO) delta 9.20 (s, 1H), 8.33 (s, 1H), 8.29 (s, 1H), 8.09 (s, 1H) |
55.2% | In ethanol; for 3.0h;Reflux; | Example 39 2'-amino-6-(6-chloroimidazo[ 1 ,2-a]pyridin-8-yl)- 1 ',2,2-trimethylspiro[chroman-4,4'- imidazol]-5'(l'H)-oneStep A: 3-Bromo-5-chloro-2-pyridinamine (487 mg, 2.35 mmol) was diluted with ethanol (4 mL), followed by the addition of 2-chloroacetaldehyde (614 , 4.69 mmol). The reaction was heated at reflux for 3 hours. The reaction was cooled and loaded onto silica gel eluting with 10-50% ethyl acetate/hexanes to yield 8-bromo-6-chloroimidazo[l,2-a]pyridine (300 mg, 1.30 mmol, 55.2% yield).Step B: 2'-Amino-r,2,2-trimethyl-6-(4,4,5,5-tetramethyl |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
34% | With sodium carbonate;tetrakis(triphenylphosphine) palladium(0); In 1,4-dioxane; at 85.0℃; for 12.0h;Sealed tube; | Step B: 2'-Amino-r,2,2-trimethyl-6-(4,4,5,5-tetramethyl-l,3,2-dioxaborolan-2-yl)spiro[chroman-4,4'- imidazol]-5'(l'H)-one (50 mg, 0.13 mmol; see Example 103, Step A) and 8-bromo-6-chloroimidazo[l,2- ajpyridine (60 mg, 0.26 mmol) were diluted with dioxane (1 mL), followed by the addition of Pd(PPh3)4 (7.5 mg, 0.0065 mmol) and Na2C03 (324 mu, 0.65 mmol). The reaction was sealed, heated to 85C and stirred for 12 hours. The reaction was loaded directly onto silica gel and eluted with 1-10% methanol/DCM (1% Nu?OmicronEta) to afford 2'-amino-6-(6-chloroimidazo[l,2-a]pyridin-8-yl)-l',2,2- trimethylspiro[chroman-4,4'-imidazol]-5'(rH)-one (18 mg, 0.044 mmol, 34% yield), m/z (APCI-pos) M+l = 410.2 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
66% | With tris-(dibenzylideneacetone)dipalladium(0); caesium carbonate; 4,5-bis(diphenylphos4,5-bis(diphenylphosphino)-9,9-dimethylxanthenephino)-9,9-dimethylxanthene; In 1,4-dioxane; at 100.0℃; | A 50-mL round-bottomed flask equipped with a reflux condenser was charged with <strong>[957187-27-8]8-bromo-6-chloroimidazo[1,2-a]pyridine</strong> 101a (264 mg, 1.14 mmol), 5-(4-(oxetan-3-yl)piperazin-1-yl)pyridin-2-amine (328 mg, 1.14 mmol), Pd2(dba)3 (102 mg, 0.11 mmol), Xantphos (63 mg, 0.11 mmol), Cs2CO3 (3.58 g, 11.0 mmol), dioxane (20 mL). After three cycles of vacuum/argon flush, the mixture was heated at 100 C. overnight. It was then filtered and the filtrate was evaporated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with 1:50 methanol/dichloromethane to afford 121a as an orange solid (290 mg, 66%). MS-ESI: [M+H]+385.1 |
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