HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Chloroethyl chloroformate → trans-4-(2,5-Dimethylpiperazin-1-yl)-2-trifluoromethylbenzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Chloroethyl chloroformate | HCID 521305 | — |
| Reactant | (2S,5R)-4-(4-Benzyl-2,5-dimethylpiperazin-1-yl)-2-trifluoromethylbenzonitrile | HCID 11639373 | — |
| Solvent | 1,1-Dichloroethane | HCID 6365 | — |
| Product | trans-4-(2,5-Dimethylpiperazin-1-yl)-2-trifluoromethylbenzonitrile | HCID 11391932 | 80.8% |
Reaction Steps
A 0.92 ml portion of 1-chloroethyl chloroformate was added to 20 ml of dichloroethane solution containing 0.31 g of (2S,5R)-4-(4-benzyl-2,5-dimethylpiperazin-1-yl)-2-trifluoromethylbenzonitrile, and the mixture was stirred for 2 days with heating under reflux. The reaction mixture was concentrated, mixed with 20 ml of methanol and then stirred for 1 day with heating under reflux. The reaction mixture was concentrated and the residue was subjected to a silica gel column chromatography and purified with chloroform-methanol (9:1, v/v) to obtain 0.19 g of the title compound as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06673799B1 |
| Source dataset | uspto-grants-2004_01 |
| ORD ID | ord-2342bc2303f14deea84f2751770ce840 |
| Source note | uspto-grants-2004_01 |