HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 3-Bromobenzophenone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Thiosemicarbazide | HCID 2723789 | — |
| Reactant | HCID 74411416 | HCID 74411416 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 3-Bromobenzophenone | HCID 70548 | 34% |
Reaction Steps
Phenyl(3-bromophenyl) ketone thiosemicarbazone (13) Into a round bottom flask containing the appropriate ketone (1.79 g, 6.84 mmol), 30 mL of anhydrous methanol were added and the solution was refluxed for about 15 minutes. To the warm ketone solution, thiosemicarbazide (0.600 g, 6.59 mmol) and 1% solution of HOAc (0.8 mL) were added. The reaction mixture was refluxed under nitrogen atmosphere for 26 h, at which point, the solvent was evaporated and, the crude reaction mixture was purified by flash chromatography (30% EtOAc/70% hex) to obtain 0.7739 g (2.32 mmol) of the product in a 34% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08173696B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-d0b1bba57aa94ac0bcf89b0adda14a0b |
| Source note | uspto-grants-2012_05 |