HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3',5'-Dichloroacetophenone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 3,5-Dichloro-N-methoxy-N-methylbenzamide | HCID 58797333 | — |
| Reactant | HCID 178418573 | HCID 178418573 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3',5'-Dichloroacetophenone | HCID 2758058 | — |
Reaction Steps
To the product from step A (5.42 g, 23.2 mmol) in 100 mL of tetrahydrofuran was added methylmagnesium bromide (11.6 mL, 34.8 mmol) drop-wise. After stirring at ambient temperature for 25 min, 1N hydrochloric acid was added and the mixture extracted with two portions of ethyl acetate. The combined organic layers were dried over magnesium sulfate and concentrated in vacuo to provide the title compound which was used without further purification. 1H NMR (500 MHz, CDCl3) δ: 7.84 (d, J=1.9 Hz, 2H); 7.58 (d, J=1.8 Hz, 1H); 2.63 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07625938B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-b57a569bbe5b4bebbd9de99fd9714405 |
| Source note | uspto-grants-2009_12 |