HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 90236513, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | trans-tert-butyl 1-benzyl-2-oxooctahydro-6H-pyrido[3,4-b][1,4]oxazine-6-carboxylate | HCID 90236047 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 90236513 | HCID 90236513 | — |
Reaction Steps
To a solution of trans-tert-butyl 1-benzyl-2-oxooctahydro-6H-pyrido[3,4-b][1,4]oxazine-6-carboxylate (126 g, 346 mmol) in anhydrous THF (2 L) was added borane methylsulfide complex (109 mL, 1.038 mol) drop wise at 0° C. The mixture was stirred at room temperature overnight. Methanol (300 mL) was added to the mixture at room temperature and heated to reflux for 1 h. The mixture was washed with saturated NaHCO3 and brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel chromatography to afford tert-butyl 1-benzyloctahydro-6H-pyrido[3,4-b][1,4]oxazine-6-carboxylate as a mixture of trans diastereomers.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846657B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-0727242ba4b74d0a813cafd8c470fa62 |
| Source note | uspto-grants-2014_09 |