HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → HCID 22458184, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | HCID 22458110 | HCID 22458110 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22458184 | HCID 22458184 | — |
Reaction Steps
A solution of 1 M boron tribromide in CH2Cl2 (2.37 mL) was dropped into another solution containing 0.74 g of 1-(N-phenyl-2-aminoethyl)-4-(2-methoxyphenyl)piperazine in 10 ml, of CH2Cl2 stirred at −3° C. in nitrogen atmosphere. Subsequently, 0.25 mL of acetonitrile at room temperature was added and the mixture was stirred for 1h at room temperature and for 8 h until precipitation. After cooling at room temperature, the mixture was treated with a 10% aqueous solution of Na2CO3 and the organic phase that separated was dried on anhydrous Na2SO4 and evaporated to dryness. The crude was purified via flash chromatography (CH2Cl2-MeOH 98:2) and the residue crystallized from EtOH giving 0.33 g (39%) of the title compound. Melting point: 92-94° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06399614B1 |
| Source dataset | uspto-grants-2002_06 |
| ORD ID | ord-2b11b6fb4c2647bfb43a7876c48c2b15 |
| Source note | uspto-grants-2002_06 |