HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetone → Ethyl 1-(2-chloroethyl)piperidine-4-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | 1-Bromo-2-Chloroethane | HCID 7849 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Ethyl nipecotate | HCID 98969 | — |
| Product | Ethyl 1-(2-chloroethyl)piperidine-4-carboxylate | HCID 61287119 | 38.6% |
Reaction Steps
To a solution of ethyl nipecotate (20.0 mL, 130 mmol) in acetone (180 mL) was added 1-bromo-2-chloroethane (21.6 mL, 260 mmol) followed by anhydrous K2CO3 (27.12 g, 196 mmol). The reaction mixture was stirred for 24 h and then concentrated under vacuum. The resulting residue was treated with H2O (75 mL) and extracted with Et2O. The combined organic layers were dried with MgSO4, filtered, and concentrated under vacuum. Purification of the crude residue by flash chromatography (50% Et2O/50% hexane) on silica gel gave the title compound (10.99 g, 38.6%). EI-MS m/z 220(M+H+) Rt (1.20 min).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08853404B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-4f9cd186fef64a0f9f35f76399c2a664 |
| Source note | uspto-grants-2014_10 |