HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68795638, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Chlorobenzenesulphonyl chloride | HCID 17909 | — |
| Reactant | 1-(1,1-Dimethylethyl) 2-methyl 1,2-piperazinedicarboxylate | HCID 2756818 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68795638 | HCID 68795638 | — |
Reaction Steps
To a solution of N-1-Boc-2-piperazinecarboxylic acid methyl ester (CAS Reg. No: [129799-15-1]) (1 g) in DMF (5 mL) was added 3-chlorobenzenesulfonyl chloride (0.95 g) and triethylamine (1.71 mL). The reaction mixture was stirred at RT overnight. Water was added and the mixture was extracted with ethyl acetate (×2). The combined organic layers were washed with water (×2) and brine, were dried (Na2SO4), filtered and evaporated. Purification by chromatography (SiO2, n-heptane/ethyl acetate 3:1) yielded 4-(3-chloro-benzenesulfonyl)-piperazine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester as white foam (1.66 g), MS: 436.3 ([M+NH4, 1Cl]+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08288541B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-81592d984c374779b75845a54ce66ea6 |
| Source note | uspto-grants-2012_10 |