Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Cyclopropanecarboxaldehyde | HCID 123114 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Reactant | HCID 68510433 | HCID 68510433 | — |
| Solvent | N,N-Dimethylformamide--water (1/1) | HCID 21962138 | — |
| Product | HCID 68510193 | HCID 68510193 | 37.2% |
Reaction Steps
To a solution of 4-(2-amino-4-methyl-phenylamino)-3-hydroxy-piperidine-1-carboxylic acid tert-butyl ester (2 g, 6.23 mmol) and cyclopropanecarboxaldehyde (485 μL, 6.5 mmol) in a 3% H2O/DMF (10 mL) solution was added Oxone® (3.05 g, 4.96 mmol). The mixture was stirred for 1 h and poured into a 0.2 N NaOH solution (25 mL). After stirring for 5 minutes, the aqueous layer was extracted four times with ethyl acetate. The combined organic extracts were washed twice with water, once with brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by flash chromatography (4/1 ethyl acetate/hexanes) to yield 4-(2-cyclopropyl-5-methyl-benzoimidazol-1-yl)-3-hydroxy-piperidine-1-carboxylic acid tert-butyl ester (860 mg, 37%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07803816B2 |
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| Source dataset | uspto-grants-2010_09 |
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| ORD ID | ord-83021569f3c9458e8cdc1ea9d2ee9b60 |
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| Source note | uspto-grants-2010_09 |
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