HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 10427600, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Epibromohydrin | HCID 18430 | — |
| Reactant | 1-(Bis(4-fluorophenyl)methyl)piperazine | HCID 152932 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 10427600 | HCID 10427600 | — |
Reaction Steps
A solution of 4,4'-difluorobenzhydrylpiperazine (28.83 g, 100 mmol) in acetonitrile (250 mL) was added to an ice cold mixture of epibromohydrin (9.1 mL, 110 mmol) and anhydrous potassium carbonate (15.2 g, 110 mmol) in acetonitrile (150 mL) over a period of 40 min. The mixture was stirred at room temperature for 100 h, filtered and the solids were washed with methylene chloride. The combined filtrates were concentrated to dryness to give an oil which was eluted through a flash chromatographic silica gel column using 2-3% methanol/methylene chloride to give the title compound as glass, 23.98 (69.6%); 300 MHz 1H NMR (CDCl3): δ 7.4-6.9 (m, 8H). 4.22 (s. 1H). 3.09 (br m, 1H), 2.8-2.25 (m, 12H); MS 345 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04876257 |
| Source dataset | uspto-grants-1989_10 |
| ORD ID | ord-e72aee59c1334f9ea4944e5d35cb3f5a |
| Source note | uspto-grants-1989_10 |