HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,1-Dimethoxyethyl(dimethyl)amine → HCID 117737325, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,1-Dimethoxyethyl(dimethyl)amine | HCID 87835 | — |
| Reactant | HCID 117737202 | HCID 117737202 | — |
| Product | HCID 117737325 | HCID 117737325 | 63.7% |
Reaction Steps
A solution of 1-(5-(benzylthio)-2-fluorophenyl)ethanone (3.6 g, 13.83 mmol) in N,N-dimethylacetamide dimethyl acetal (12.13 mL, 83 mmol) was irradiated at 130° C. for 10 minutes in a microwave reactor (Biotage Initiator). The reaction mixture was partitioned between water and ethyl acetate, and the organic layer was concentrated. The crude product was purified by column chromatography, eluting with 20-100% ethyl acetate in heptane, to provide (E)-1-(5-(benzylthio)-2-fluorophenyl)-3-(dimethylamino)but-2-en-1-one (2.9 g, 8.80 mmol, 63.7% yield) as a tan solid. m/z (ESI) 330.0 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09212182B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-98e078cd17cb493891b39c75480ad14c |
| Source note | uspto-grants-2015_12 |