HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 21689652, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Epichlorohydrin | HCID 7835 | — |
| Reactant | 1-(Bis(4-fluorophenyl)methyl)piperazine | HCID 152932 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 21689652 | HCID 21689652 | 100.8% |
Reaction Steps
[Bis(4-fluorophenyl)methyl]piperazine, (14.4 g, 0.05 mol) in ethanol (200 mL) was added dropwise to epichlorohydrin (3.5 mL, 0.05 mol) in ethanol (12 mL) at 0° C. with NaHCO3 anhydrous (4.2 g, 0.05 mol) over 45 min under N2. The ice bath was removed and the mixture was allowed to come to room temperature. After 18 h the NaHCO3 was removed by fitration via a sintered glass funnel and the ethanol in the fitrate was removed in vacuo to give the crude product (21.3 g). Flash chromatography over silica gel using 2.0% methanol: methylene chloride gave pure product (10.05 g, 52.9%) as an amber oil. DCI/MS (M+1)381.400 MHz 1H NMR (CDCl3) δ: 7.3 (m,4H), 6.95 (m,4H), 4.2 (s, 1H), 3.95(m,1H),3.55(m,2H),2.7 (m,2H), 2.5(m,4M), 2.4 (m, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | USRE035072 |
| Source dataset | uspto-grants-1995_10 |
| ORD ID | ord-d2c43a16c0104237bfbb466caaeca969 |
| Source note | uspto-grants-1995_10 |