HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 22010658, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Carbon tetrabromide | HCID 11205 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 22010692 | HCID 22010692 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 22010658 | HCID 22010658 | 92.1% |
Reaction Steps
To a solution of 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-(3-hydroxypropoxy)phenyl]benzamide (520 mg) in dichloromethane (20 ml) was added triphenylphosphine (827 mg) and carbon tetrabromide (1.39 g) at ambient temperature. The mixture was stirred for 2 hours and diluted with ethyl acetate and washed successively with saturated sodium hydrogen carbonate and brine, and dried over magnesium sulfate. The solid was removed and the solvent was removed by evaporation to give crude product. The crude material was subjected to a silica gel column chromatography (SiO2; 50 g, 0.5% methanol in chloroform) to give 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-(3-bromopropoxy)phenyl]benzamide (540 mg) as white amorphous.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06211242B1 |
| Source dataset | uspto-grants-2001_04 |
| ORD ID | ord-5283998ff2e04f658d8a935b02749ab8 |
| Source note | uspto-grants-2001_04 |