HuagongsheHuagongshe Chemistry Print Report · For research reference only
Oxalic Acid → HCID 25143957, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Oxalic Acid | HCID 971 | — |
| Reactant | 1-Bromo-2-methylpropane | HCID 6555 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 63585886 | HCID 63585886 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 25143957 | HCID 25143957 | — |
Reaction Steps
Preparation according to Example 51. Enantiomer E1 of 3-(3,5-difluorophenyl)-pyrrolidin-3-ol (0.18 g, 0.92 mmol), acetonitrile (6 mL), potassium carbonate (0.25 g, 1.84 mmol), 1-bromo-2-methylpropane (0.1 mL, 0.92 mmol). Flash chromatography on silica gel (ethyl acetate/methanol, 9:1). Yield: 0.18 g. [α]D=+22.6° (methanol). The amine was converted to the oxalic acid salt and recrystallized from methanol/diisopropyl ether: M.p. 164-165° C.; MS m/z (relative intensity, 70 eV) 255 (M+, 2), 212 (bp), 182 (46), 213 (12), 127 (8), 98 (6) 1-bromo-2-methylpropane.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08188301B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-75794111d9e24b41a9afcc0623673e29 |
| Source note | uspto-grants-2012_05 |