Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydroxylamine | HCID 787 | — |
| Reactant | Ethyl 2-cyanopropionate | HCID 98018 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 133681488 | HCID 133681488 | — |
Reaction Steps
Ethyl 2-methylcyanoacetate (5 g, 39 mmol) and hydroxylamine (2.6 g, 39 mmol) were dissolved in 50 mL of MeOH. The solution was heated at the 50° C. overnight. The solution was then concentrated and the residue purified by silica gel chromatography using a hexanes/EtOAc gradient to give the indicated product. 1H NMR δ (ppm) (DMSO-d6): 9.05 (1H, s), 5.40 (2H, s), 4.06 (2H, dd, J=12.8, 7.0 Hz), 3.15 (1H, m), 1.24 (3H, d, J=7.2 Hz), 1.18 (3H, t, J=7.1 Hz). m/z=161.1 (M+H)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09365574B2 |
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| Source dataset | uspto-grants-2016_06 |
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| ORD ID | ord-f7d590db05bb4515859da1a703ef0b5a |
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| Source note | uspto-grants-2016_06 |
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