HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 68682042, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl diethoxyacetate | HCID 80169 | — |
| Reactant | 3',5'-Difluoroacetophenone | HCID 518596 | — |
| Reactant | LiHMDS tetrahydrofuran | HCID 23714775 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68682042 | HCID 68682042 | — |
Reaction Steps
At −78° C., a tetrahydrofuran (20 ml) solution of 3,5-difluoroacetophenone (8.86 g) was added to a tetrahydrofuran (180 ml) solution of 1 N lithium hexamethyldisilazide/tetrahydrofuran solution (68 ml), and stirred at the same temperature for 1 hour. At −78° C., ethyl diethoxyacetate (12.2 ml) was added to the reaction liquid, and stirred overnight at room temperature. At 0° C., 2 N hydrochloric acid (60 ml) was added to the reaction liquid, and extracted with ethyl acetate. The extract was washed with saturated saline water, dried with anhydrous magnesium sulfate, and the solvent was evaporated off to obtain the entitled compound (16.5 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07829586B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-4730720d2d194d4081209c9dd3305e27 |
| Source note | uspto-grants-2010_11 |