HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 118020440, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium borohydride | HCID 4148881 | — |
| Reactant | HCID 118201023 | HCID 118201023 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 118020440 | HCID 118020440 | — |
Reaction Steps
To a solution of (±)-ethyl 3-[5-methyl-2-(2H-1,2,3-triazol-2-yl)benzoyl]-1,3-oxazinane-2-carboxylate obtained in Reference Example 3 (0.50 g, 1.5 mmol) in THF (5 mL), a solution of LiBH4 in THF (0.97 mL, 2.9 mmol) was added and stirred for 2 hours at room temperature. Water was added to the reaction mixture, followed by extraction with CHCl3. The organic layer was washed with a saturated aqueous solution of sodium chloride, dried over Na2SO4, then the drying agent was filtered off, and then the solvent was distilled off under reduced pressure. The obtained residue was purified by column chromatography (HP-Sil 25 g, hexane/EtOAc=88/12 to 0/100) to obtain the title compound (0.34 g) (colorless oil).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09266870B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-e8cf2fa105624e67adf7701e9cbcaffa |
| Source note | uspto-grants-2016_02 |