HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 63936931, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Piperidin-4-ol | HCID 79341 | — |
| Reactant | Tetrahydro-4H-pyran-4-one | HCID 121599 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Titanium isopropoxide | HCID 11026 | — |
| Product | HCID 63936931 | HCID 63936931 | — |
Reaction Steps
Piperidin-4-ol (7.8 g) and dihydro-2H-pyran-4(3H)-one (5.0 g) were dissolved in titanium(IV) isopropoxide (30 mL) and the reaction was stirred at room temperature overnight. Methanol (40 mL) was added and the reaction was cooled to 0° C. Then NaBH4 (3.8 g) was added in portions over one hour. After 2 hours 1N aqueous NaOH was added, followed by ethyl acetate addition. After filtration though celite the layers were separated, the aqueous layer extracted with ethyl acetate, and the combined organic layers were dried over Na2SO4. The crude was purified by column chromatography using dichloromethane having 5-10% 7N NH3 in methanol.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08546399B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-b17463474fa7444e946affb273bab312 |
| Source note | uspto-grants-2013_10 |