Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 86615035 | HCID 86615035 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23156199 | HCID 23156199 | 23% |
Reaction Steps
Under argon atmosphere, a solution of aluminum trichloride (0.136 g, 1.02 mmol) in THF (2.5 mL) was dropped into a solution of lithium aluminum hydride (77.4 mg, 2.04 mmol) in THF (3.0 mL) at 0° C. Then, a solution of 1-methylpiperidine-4-carboxylic acid [4-(2,5,7-trimethyl-3H-imidazo[4,5-b]pyridin-3-ylmethyl)phenyl amide] (1.53 g, 3.31 mmol) obtained in Step 1 in THF (3.0 mL) was dropped into the mixture. The mixture was stirred at 0° C. for 15 minutes, then at room temperature for 1.5 hours. The reaction mixture was added with a 2 mol/L aqueous sodium hydroxide solution and extracted with ethyl acetate three times. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, then concentrated under reduced pressure. The obtained crystals were recrystallized from ethanol-diisopropyl ether to obtain Compound 159 (44.3 mg, 0.12 mmol, 23%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08507484B2 |
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| Source dataset | uspto-grants-2013_08 |
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| ORD ID | ord-dede09a1d5be41f2963c89477b019d3b |
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| Source note | uspto-grants-2013_08 |
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