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 | 99.2% |
Reaction Steps
To a solution of lithium aluminum hydride (347 mg) in diethyl ether (30 mL) was added, under a nitrogen stream, aluminum(III) chloride (406 mg) at room temperature, and the mixture was stirred at room temperature for 30 min. The reaction mixture was cooled to −78° C., a solution of (6RS,7RS)-4-benzyl-6-({[tert-butyl(dimethyl)silyl]oxy}methyl)-7-(3,4-dichlorophenyl)-1,4-oxazepan-3-one (2.51 g) in THF (20 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 (5 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 (2.42 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08722662B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-b5e067eafaf84aa5856346f075872a38 |
| Source note | uspto-grants-2014_05 |