HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 66955253, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Chlorotrimethylsilane | HCID 6397 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Tert-butyl 3-cyano-3-(trimethylsilyloxy)piperidine-1-carboxylate | HCID 58374194 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 66955253 | HCID 66955253 | — |
Reaction Steps
tert-Butyl 3-cyano-3-(trimethylsilyloxy)piperidine-1-carboxylate, Preparation 34A (170 mg, 0.570 mmol) was treated with 6N HCl in MeOH (10 mL) at 80° C. for 12 hours. Solvents were removed in vacuo and the resulting material was dissolved in MeOH (10 mL). HCl (g) was bubbled through the mixture for 15 minutes. The solids were concentrated in vacuo. The residue was dissolved in DCM (10.00 mL) and cesium carbonate (928 mg, 2.85 mmol) was added. Next, TMS—Cl (0.146 mL, 1.139 mmol) was added and the mixture was stirred for 1 hour. The mixture was filtered and the solids were concentrated in vacuo and taken to the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08399451B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-5e18151ba7b7423fb6a52dcf8095f488 |
| Source note | uspto-grants-2013_03 |