HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → Bis(3-bromophenyl)methanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Thiosemicarbazide | HCID 2723789 | — |
| Reactant | 1-(Bis(3-bromophenyl)methylene)thiosemicarbazide | HCID 16061497 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | Bis(3-bromophenyl)methanone | HCID 12731928 | 18% |
Reaction Steps
Bis(3-bromophenyl) ketone thiosemicarbazone (14) Into a round bottom flask containing the appropriate ketone (1.044 g, 3.07 mmol), 35 mL of anhydrous methanol were added and the solution was refluxed for about 15 minutes. To the warm ketone solution, thiosemicarbazide (0.294 g, 3.23 mmol) and 1% solution of HOAc (1.5 mL) were added. The reaction mixture was refluxed under nitrogen atmosphere for 46 h, at which point, the solvent was evaporated and, the crude reaction mixture was purified by flash chromatography (20% EtOAc/80% hex) to obtain 0.231 g (0.559 mmol) of the product in an 18% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08173696B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-2bafa9ee83dc4b2f9e782c9aa00a7a7d |
| Source note | uspto-grants-2012_05 |