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CAS No. : | 6601-22-5 | MDL No. : | MFCD00460178 |
Formula : | C7H8Cl2N4O | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | UQAMDAUJTXFNAD-UHFFFAOYSA-N |
M.W : | 235.07 | Pubchem ID : | 81076 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280-P305+P351+P338-P310 | 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 |
---|---|---|
With N-ethyl-N,N-diisopropylamine; In tetrahydrofuran; at 20℃; for 16h; | 4-Phenoxypiperidine (0.15g) was added to a solution of the product from step (i) (0.2g), [N,] N-diisopropylethylamine (1. [47ML)] in tetrahydrofuran and stirred at room temperature for 16h. The solvent was evaporated under reduced pressure and the residue purified by chromatography on silica eluting with ether/isohexane (1: 2). Yield 0.3g white solid. The solid was dissolved in N, [N-DIMETHYLFORMAMIDE] [(20ML),] sodium cyanide [(0.] lg) added and heated at [90C] for 32h. The mixture was partitioned between ethyl acetate and water, the organic layer separated, washed with water, brine, dried (MgS04) and evaporated under reduced pressure. The residue was purified by RPHPLC 35-95% acetonitrile in aqueous [TRIFLUOROACETIC] acid. Yield 0.079g MS: APCI (+ve) 367 (+H) [1HNMR] : (DMSO-d6) 8 7.31-6. 91 (5H, [M),] 4.66 [(1H,] [M),] 4.11-4. 04 (2H, [M),] 3.70- 3.57 [(10H,] [M),] 2.00-1. 95 (2H, m), 1.63-1. 60 (2H, [M)] |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
99% | With triethylamine; In water; acetone; at 20℃; for 6h; | To a stirred acetone/crushed ice suspension of 2,4-dichloro-6-morpholin-4-yl-[1,3,5]triazine (1.5 g, 6.5 mmol), 8-oxa-3-azabicyclo[3.2.1]octane (980 mg, 6.5 mmol) and triethylamine (3 ml) was added and stirred at room temperature for 6 h. At the end, the separated solid was filtered and washed with water. The crude product was found to be pure enough for further transformations. Yield: 2.0 g (99%); mp. 118; (M+H) 313.1. |
99% | With triethylamine; In water; acetone; at 20℃; for 6h; | To a stirred acetone/crushed ice suspension of 2,4-dichloro-6-morpholin-4-yl-[1,3,5]triazine (1.5 g, 6.5 mmol), 8-oxa-3-azabicyclo[3.2.1]octane (980 mg, 6.5 mmol) and triethylamine (3 ml) was added and stirred at room temperature for 6 hours. At the end, the separated solid was filtered and washed with water. The crude product was found to be pure enough for further transformations. Yield: 2.0 g (99%); mp. 118; (M+H) 313.1 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
31% | With palladium diacetate; caesium carbonate; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene; In 1,4-dioxane; at 100℃; for 4h;Inert atmosphere; | A round bottom flask was charged with compound i11 (5.37 g, 22.9 mmol, 1 .5 eq), <strong>[109-11-5]morpholine-3-one</strong> (1 .54 g, 15.3 mmol, 1 .0 eq), 4,5-bis(diphenylphosphino)-9,9- dimethylxanthene (530 mg, 0.915 mmol, 0.06 eq.), cesium carbonate (9.95 g, 30.5 mmol, 2.0 eq) and palladium(ll) acetate (383 mg, 0.170 mmol, 0.04 eq.). The reaction mixture was flushed with nitrogen and 1 ,4-dioxane (100 mL) was added. The reaction mixture was stirred at reflux (100 C) for 4 hours. The reaction mixture was cooled to room temperature and filtered. The filter cake was washed with dichloromethane (2x 30 mL). Solvents were removed under reduced pressure and the crude product was purified using silica gel chromatography (cyclohexane / ethyl acetate 1 :0 -> 1 :3) to yield the title compound i31 as a colorless solid (390 mg, 31 %). 1H NMR (400 MHz, CDCI3): δ 4.32 (s, 2 H), 4.03-3.97 (m, 4 H), 3.93-3.86 (m, 4 H), 3.75-3.73 (m, 4 H); MS (MALDI): m/z = 299.6 M+H]+). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
46% | With triethylamine; In tetrahydrofuran; at 0 - 20℃; for 1h; | To a solution of the 3-aminomethyl-azetidine-1-carboxylic acid tert-butyl ester HCl salt (945 mg, 4.24 mmol) and NEt3 (856 mg, 8.48 mmol) in THF (10 mL) at 0° C. was added a suspension of 2,4-dichloro-6-morpholin-4-yl-[1,3,5]triazine (996 mg, 4.24 mmol) at 0° C. The reaction mixture was stirred for another 1 hr at 0° C. and allowed to warm to 20° C. and stirred for 1-4 hrs to drive the reaction to completion. Silica gel (20 g) was added to the reaction mixture and the solvent was removed so that product was adsorbed on the silica gel. The silica gel plug was placed on top of a column to purify by flash chromatography using CH2Cl2/ MeOH/ NH3 (20:1:01) eluent. After unifying the product fraction, and evaporation of solvent, (750 mg, 46percent yield) product was obtained as yellow solid; MS (ESI) m/z 385 |
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