HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 69411481, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Chloropropanesulphonyl chloride | HCID 15410 | — |
| Reactant | tert-Butyl 4-(2-aminophenyl)piperazine-1-carboxylate | HCID 2795530 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69411481 | HCID 69411481 | 93.5% |
Reaction Steps
To a solution of N-boc-4-(2-amino-phenyl)-piperazine (555 mg, 2.0 mmol) and Et3N (837 uL, 6 mmol) in 20 mL of CH2Cl2 was added 3-chloropropanesulfonyl chloride (255 uL, 2.1 mmol). After stirring for about 30 minutes, the mixture was quenched with saturated aqueous sodium bicarbonate, diluted with EtOAc, washed with 1 M HCl, water and brine, and then dried (Na2SO4), filtered and concentrated. Purification by silica gel chromatography (35 g SiO2, 10 to 30% EtOAc/hexanes, over 30 min at 35 mL/min) afforded about 781 mg (1.87 mmol, 93%) of N-boc-4-[2-(3-chloro-propane-1-sulfonylamino)-phenyl]-piperazine as a white solid. LRMS (ESI+): 418.1 [M+1]
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07291619B2 |
| Source dataset | uspto-grants-2007_11 |
| ORD ID | ord-6258873b2bf2483dade7141306e93150 |
| Source note | uspto-grants-2007_11 |