HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → Tert-butyl 3-(3-chloro-5-fluorophenyl)-3-methoxypyrrolidin-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Tert-butyl 3-(3-chloro-5-fluorophenyl)-3-hydroxypyrrolidine-1-carboxylate | HCID 67402932 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Tert-butyl 3-(3-chloro-5-fluorophenyl)-3-methoxypyrrolidin-1-carboxylate | HCID 67402360 | 71.4% |
Reaction Steps
Preparation according to Preparation 2. Tert-butyl-3-(3-chloro-5-fluorophenyl)-3-hydroxypyrrolidin-1-carboxylate (2.1 g, 6.67 mmol) in dry tetrahydrofuran (50 mL), sodium hydride (60% dispersion in mineral oil, 0.40 g, 10 mmol), iodomethane (0.83 mL, 13.3 mmol). Purification by flash column chromatography on silica gel (ethyl acetate/isooctane, 1:9 to 1:1) gave the title compound (1.57 g, 71%). MS m/z (rel. intensity, 70 eV) 275 (33), 273 (bp), 256 (42), 228 (32), 57 (77).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09035073B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-56ebb72d106c483bafbdf3b6191dd288 |
| Source note | uspto-grants-2015_05 |