HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,3-Dimethylbutanal → HCID 57656530, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,3-Dimethylbutanal | HCID 76335 | — |
| Reactant | HCID 57656516 | HCID 57656516 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 57656530 | HCID 57656530 | 14.1% |
Reaction Steps
Add butyllithium (8.2 mL, 13.1 mmol) to a solution of 4-bromo-3-chloro-N-(tert-butoxycarbonyl)-benzylamine (1.823 g, 5.7 mmol) in diethyl ether (46 mL) at −78° C. under nitrogen and stir for 30 min. Add 3,3-dimethylbutyraldehyde (1.427 g, 1.7 mL, 14.3 mmol), stir for 30 min at −78° C. and then warm to room temperature. Add water and extract twice the aqueous phase with EtOAc. Dry the combined organic extracts over Na2SO4, filter and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (4:1) to obtain the desired intermediate as a yellow oil (274 mg, 14%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08580780B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-cf2f4578005040ae970d6c59442c7d5b |
| Source note | uspto-grants-2013_11 |