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CAS No. : | 160033-52-3 | MDL No. : | MFCD11111135 |
Formula : | C11H19NO4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | BSAYEGDCKUEPNE-SFYZADRCSA-N |
M.W : | 229.27 | Pubchem ID : | 10944233 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H317 | 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 |
---|---|---|
188 mg | With pyridine; trichlorophosphate; In dichloromethane; at 0℃; for 4h; | In a pre-dried flask, (2S,5 S)? 1-(tert-butoxycarbonyl)-4-methylpyrrolidine-2-carboxylic acid (230 mg, 1.0 mmol), <strong>[89466-16-0]6-bromo-3-methylpyridin-2-amine</strong> (188 mg, 1.0 mmol) are placed, and then anhydrous DCM (15 mL) was added. The flask was placed in an ice bath. To the solution, dry pyridine (0.25 mL, 3.0 mmol) was added in one portion, followed by addition of POCl3(100 muL, 1.0 mmol). After completion of addition, the mixture was stirred for 4 hours at 0° C., and then the reaction was quenched with water (15 mL). The DCM layer was collected and the aqueous phase was extracted with DCM (15 mL×2). The combined DCM solution was washed with brine, and dried over MgSO4. The solution was filtered and concentrated; the resulting residue was purified to give 188 mg pure product.1H NMR (400 MHz, DMSO-d6): (major rotamer) delta 1.12 (t, J=8.8 Hz, 3H), 1.34 (s, 9H), 1.46-1.55 (m, 1H), 1.84-1.91 (m, 1H), 2.02-2.08 (m, 1H), 2.11 (s, 3H), 2.28-2.37 (m, 1H), 3.95-4.02 (m, 1H), 4.35 (t, J=8.8 Hz, 1H), 7.43 (d, J=7.6 Hz, 1H), 7.62 (t, J=7.6 Hz, 1H), 10.26 ppm. LC (method A): tR=2.10 min. LC/MS (EI) m/z: [M+H]398.25 |
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