HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butyl 4-oxopiperidine-1-carboxylate → Tert-butyl 4-hydroxypiperidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butyl 4-oxopiperidine-1-carboxylate | HCID 735900 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Tert-butyl 4-hydroxypiperidine-1-carboxylate | HCID 643502 | 101.4% |
Reaction Steps
Sodium borohydride (3.8 g, 100.4 mmol) was added in portions to a solution of tert-butyl 4-oxo-1-piperidinecarboxylate (20 g, 100.4 mmol) in methanol (600 mL) at 0° C. After 15 minutes, the ice-water bath was removed and the reaction mixture was stirred at room temperature for 3 hours. Sodium hydroxide (1.0 N, 100 mL) was added and the organic solvent was evaporated. The aqueous was extracted with ether four times. The combined organic layer was washed with water then brine, dried over MgSO4, filtered and evaporated to give tert-butyl 4-hydroxy-1-piperidinecarboxylate (20.48 g, 100%). 1H NMR (CDCl3-d) δ 1.48 (s, 9H), 1.63 (m, 2H), 1.87 (m, 2H), 3.03 (m, 2H), 3.83 (m, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06921763B2 |
| Source dataset | uspto-grants-2005_07 |
| ORD ID | ord-9936cc68ae10426bae891d89ff9bfba8 |
| Source note | uspto-grants-2005_07 |