HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 2-methyl-3-(N-Boc-piperidine-4-yl)-propionic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Methyl N-Boc-4-piperidinepropionate | HCID 1502093 | — |
| Reactant | Sodium bis(trimethylsilyl)amide | HCID 2724254 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-methyl-3-(N-Boc-piperidine-4-yl)-propionic acid methyl ester | HCID 59261070 | — |
Reaction Conditions
| Temperature | -78 °C |
|---|
Reaction Steps
3-(N-Boc-piperidine-4-yl)-propionic acid methyl ester (2.0 g, 7.38 mmol) from above was dissolved in tetrahydrofuran (50 mL). The solution was cooled to −78° C. and sodium bis(trimethylsilyl)amide (1.0 M, 9.0 mL) was added. The mixture was stirred at −78° C. for 1 hr and methyl iodide (1.2 mL, 19.5 mmol) was added. The mixture was warmed to room temperature and stirred for 2 hrs. The mixture was extracted with ether and washed with dilute hydrochloric acid. The organic layer was dried, filtered and concentrated. The residue was purified using flash chromatography (eluting with ethyl acetate and hexanes) to give 2-methyl-3-(N-Boc-piperidine-4-yl)-propionic acid methyl ester as an oil (789 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08153644B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-9a4deedac40b4f63a9c1bcdeb98616a8 |
| Source note | uspto-grants-2012_04 |