Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cyclohexanone | HCID 7967 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | ethyl (2E)-3-(6-{(tert-butoxycarbonyl)[(3R)-3-pyrrolidinyl]amino}-3-pyridyl)acrylate dihydrochloride | HCID 86603639 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86603755 | HCID 86603755 | 129.3% |
Reaction Steps
To a mixture of ethyl (2E)-3-(6-{(tert-butoxycarbonyl)[(3R)-3-pyrrolidinyl]amino}-3-pyridinyl)acrylate dihydrochloride (256 mg) and cyclohexanone (64 mg) in 1,2-dichloroethane (5 mL) was added sodium triacetoxyborohydride (253 mg) and N,N-diisopropylethylamine (0.21 mL), and the mixture was stirred at room temperature for 2 hours. To the resultant was added saturated aqueous ammonium chloride and ethyl acetate, and the mixture was stirred for 20 min. The organic phase was separated, washed with brine and dried over Na2SO4, filtered, and concentrated in vacuo. The residue was purified by silica gel column chromatography (chloroform/methanol=95/5 v/v) to give ethyl (2E)-3-(6-{(tert-butoxycarbonyl)[(3R)-1-cyclohexyl-3-pyrrolidinyl]amino}-3-pyridinyl)acrylate (338 mg) as a pale yellow foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07557127B2 |
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| Source dataset | uspto-grants-2009_07 |
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| ORD ID | ord-bd04a0b3ed7744c2932e97b2fe5b5b68 |
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| Source note | uspto-grants-2009_07 |
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