HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butyl piperazine-1-carboxylate → HCID 22467481, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Reactant | 2-Fluoro-5-chlorosulfonylbenzoic acid | HCID 608984 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22467481 | HCID 22467481 | 69.4% |
Reaction Steps
5-Chlorosulfonyl-2-fluorobenzoic acid (2 g) was dissolved in dichloromethane (20 mL) under nitrogen atmosphere and cooled to 0° C. tert-Butyl 1-piperazinecarboxylate (3.12 g) was added portionwise to the solution at 0° C. and stirred for 3 hours at ambient temperature. The organic solvent was evaporated in vacuo, and the residue was dissolved in 1N-sodium hydroxide solution. The aqueous solution was washed with diethyl ether and acidified with 1N-hydrochloric acid. The precipitates were collected by filtration and washed with water to give 5-[4-(tert-butoxycarbonyl)piperazin-1-ylsulfonyl]-2-fluorobenzoic acid (2.26 g) as a colorless solid substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06384080B1 |
| Source dataset | uspto-grants-2002_05 |
| ORD ID | ord-2eb25892942849d8a8116fad9ed8c904 |
| Source note | uspto-grants-2002_05 |