HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 118939068, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | n-Butyl lithium | HCID 61028 | — |
| Reactant | N-((1S)-1-(4-Bromophenyl)ethyl)acetamide | HCID 793484 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 118939068 | HCID 118939068 | — |
Reaction Steps
To 20.0 g (74.3 mmol) (S)—N-(1-(4-bromophenyl)ethyl)acetamid (WO 2012/01107) in 300 mL THF are added dropwise 75.0 mL (187 mmol)N-butyllithium (2.5 M in THF) at −78° C. and stirred for 1 h. 10.0 mL (124 mmol) DMF are added dropwise to the mixture at −78° C. and stirred for 2 h. After that aq. NH4CI solution is added and extracted with EtOAc. The organic layer is dried over Na2SO4, filtered and concentrated by evaporation. The residue is purified by column chromatography (silica gel, MeOH:DCM).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09340510B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-7a546480212a47d59db3e05d4054172c |
| Source note | uspto-grants-2016_05 |