HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisobutylaluminum hydride → Tert-butyl 2-hydroxy-1-((phenylthio)methyl)ethylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisobutylaluminum hydride | HCID 14487 | — |
| Reactant | Methyl n-(tert-butoxycarbonyl)-s-phenylcysteinate | HCID 18637399 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Tert-butyl 2-hydroxy-1-((phenylthio)methyl)ethylcarbamate | HCID 13969831 | — |
Reaction Steps
A solution of Example 175A (1.22 g, 3.91 mmol) in toluene (10 mL) at −78° C. was treated with 1M DIBAL-H in toluene (8.6 mL), warmed to room temperature over 4 hours, diluted with ethyl acetate (100 mL), washed sequentially with 0.1N HCl (30 mL), water (15 mL), and brine (50 mL), dried (MgSO4), filtered, and concentrated. The concentrate was purified by flash column chromatography on silica gel with 30% ethyl acetate/hexanes to provide the desired product. MS (DCI) m/e 284 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07504512B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-d538eb01bc4842b685617d6d5a94c62a |
| Source note | uspto-grants-2009_03 |