HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → Tert-butyl 4-[4-(hydroxymethyl)-1,3-thiazol-2-yl]piperidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl 2-(1-(tert-butoxycarbonyl)piperidin-4-yl)thiazole-4-carboxylate | HCID 2795532 | — |
| Reactant | Lithium borohydride | HCID 4148881 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | Tert-butyl 4-[4-(hydroxymethyl)-1,3-thiazol-2-yl]piperidine-1-carboxylate | HCID 7164573 | — |
Reaction Steps
A mixture of 1,1-dimethylethyl 4-[4-(ethoxycarbonyl)-2-thiazolyl]-1-piperidinecarboxylate (i.e. the product of Example 1, Step A) (3.4 g, 10 mmol), lithium borohydride (0.33 g, 15 mmol) and methanol (607 μL, 15 mmol) in diethyl ether (40 mL) was heated at reflux for 16 h. The reaction mixture was cooled, treated with water (5 mL) and extracted with diethyl ether and dichloromethane. The combined organic layers were dried (MgSO4) and concentrated under reduced pressure and purified by silica gel chromatography using 50-100% ethyl acetate in hexanes as eluant to give 1.72 g of the title compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08084468B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-8505d73bb2a54c3d9e2e1b6cf1a0774b |
| Source note | uspto-grants-2011_12 |