Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 2-Methyl-2-butene | HCID 10553 | — |
| Reactant | Sodium Chlorite | HCID 23668197 | — |
| Reactant | Sodium Phosphate, Monobasic, Dihydrate | HCID 23673460 | — |
| Reactant | HCID 72338934 | HCID 72338934 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68625833 | HCID 68625833 | 98.9% |
Reaction Steps
5-Benzyl-5-formyl-hexahydro-cyclopenta[c]pyrrole-2-carboxylic acid dimethylamide 14b (0.729 g, 2.43 mmol) was dissolved in the solvent mixture of 28 mL of tetrahydrofuran and 14 mL of water under nitrogen atmosphere, followed by addition of sodium dihydrogenphosphate dihydrate (1.14 g, 7.29 mmol), sodium chlorite (0.66 g, 7.29 mmol) and 2-methyl-2-butene (0.513 g, 7.32 mmol) upon cooling to 0° C. The reaction mixture was stirred at 0° C. for 2 hours. The reaction was monitored by TLC until the disappearance of the starting materials. The mixture was extracted with ethyl acetate. The combined organic extracts were dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography to obtain the title compound 5-benzyl-2-dimethylcarbamoyl-octahydro-cyclopenta[c]pyrrole-5-carboxylic acid 14c (0.76 g, yield 98%) as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08415349B2 |
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| Source dataset | uspto-grants-2013_04 |
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| ORD ID | ord-93309030dcac43c9a43bd80836673512 |
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| Source note | uspto-grants-2013_04 |
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