HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 66649293, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | p-(Trifluoromethoxy)benzenesulphonyl chloride | HCID 523102 | — |
| Reactant | (R)-1-Boc-3-methylpiperazine | HCID 2756811 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66649293 | HCID 66649293 | — |
Reaction Steps
To a solution of 1,1-dimethylethyl(3R)-3-methyl-1-piperazinecarboxylate (605 mg, 2.56 mmol) in DCM (20 ml) was added DIPEA (1.12 ml, 6.39 mmol) and then portionwise 4-[(trifluoromethyl)oxy]benzenesulfonyl chloride (0.455 ml, 2.68 mmol) at room temp and the resultant mixture stirred under Ar for 16 h. DCM (75 ml) and a 1M HCl solution (75 ml) were added, the layers were separated and the organic layer was then washed with 2M NaOH solution (75 ml), the organic layers were separated, dried (MgSO4) and concentrated to dryness. 1,1-Dimethylethyl(3R)-3-methyl-4-({4-[(trifluoromethyl)oxy]phenyl}sulfonyl)-1-piperazinecarboxylate was isolated as a slowly crystallizing white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08093249B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-54f706a22a2144fd9d97ce541b5e2567 |
| Source note | uspto-grants-2012_01 |