Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 67152512 | HCID 67152512 | — |
| Product | HCID 59843349 | HCID 59843349 | — |
Reaction Steps
To 3-{1-[7-(4-bromo-2,6-dimethyl-phenyl)-2,5,6-trimethyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl]-piperidin-4-yl}-propionitrile (0.40 g), H2SO4 (4 mL) was added and the mixture was stirred at room temperature for 5 hours. The reaction mixture was poured into ice, and then was made to alkaline by adding 4 M aqueous NaOH solution. The mixture was extracted with ethyl acetate and the organic phase and the organic phase was dried over Na2SO4. The desiccant was removed by filtration and the filtrate was concentrated under reduced pressure. The residue was purified with column chromatography (silica gel: Wako gel C200, eluent: CHCl3:methanol=60/1) to obtain an oil. The oily product was crystallized from diethylether to obtain the title compound (0.33 g) as a white crystal.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07951811B2 |
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| Source dataset | uspto-grants-2011_05 |
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| ORD ID | ord-e3d2275bd32d4e1d9cf4321aecd542e2 |
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| Source note | uspto-grants-2011_05 |
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