HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Boc-piperidine-3-carboxaldehyde → Tert-butyl 3-(2-methoxyethenyl)-1-piperidinecarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Boc-piperidine-3-carboxaldehyde | HCID 9964448 | — |
| Reactant | (Methoxymethyl)phosphonium chloride | HCID 22258747 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Tert-butyl 3-(2-methoxyethenyl)-1-piperidinecarboxylate | HCID 69249758 | 48.1% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a suspension of methoxymethylphosphonium chloride (5.14 g, 15 mmol) in THF (18 mL) was added potassium tert-butoxide (1.98 g, 15 mmol) at 0° C., and the mixture was stirred at 0° C. for 0.5 hr. A solution of tert-butyl 3-formyl-1-piperidinecarboxylate (2.13 g, 10 mmol) in THF (8 mL) was added dropwise at −20° C., and the resulting mixture was stirred at 0° C. to room temperature overnight. The mixture was partitioned between toluene and water. The separated organic phase was washed with brine, dried over Na2SO4, filtered, and evaporated. Purification by column chromatography on silica gel (hexane/ethyl acetate=5/1) gave tert-butyl 3-(2-methoxyethenyl)-1-piperidinecarboxylate as a colorless oil (1.16 g, yield; 48%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06562811B1 |
| Source dataset | uspto-grants-2003_05 |
| ORD ID | ord-1dffa717139d4b668c4deb08a12b7fe3 |
| Source note | uspto-grants-2003_05 |