HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 66975115, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 66974911 | HCID 66974911 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66975115 | HCID 66975115 | 93.1% |
Reaction Steps
To a solution of lithium aluminum hydride (1.49 g) in diethyl ether (120 mL) was added, under a nitrogen stream, aluminum(III) chloride (1.74 g) under ice-cooling, and the mixture was stirred at room temperature for 40 min. The reaction mixture was cooled to −78° C., a solution of (6RS,7SR)-4-benzyl-6-({[tert-butyl(dimethyl)silyl]oxy}methyl)-7-(3,4-dichlorophenyl)-1,4-oxazepan-3-one (10.8 g) in THF (80 mL) was added dropwise, and the mixture was stirred at 0° C. for 3 hr. To the reaction mixture was added 1 N aqueous sodium hydroxide solution (22 mL) at −78° C., and the mixture was stirred at room temperature for 2 hr, and filtered through celite. The filtrate was concentrated under reduced pressure to give the title compound (9.77 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08722662B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-2293c8d4f79b4fab9439756951da827b |
| Source note | uspto-grants-2014_05 |