HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methylpiperazine → HCID 21254959, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | HCID 21255002 | HCID 21255002 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21254959 | HCID 21254959 | 69% |
Reaction Steps
0.33 ml (3 mmol) of 1-methyl-piperazine in 5 ml of DMF was added to a solution of 0.50 g (1.2 mmol) of 3-benzenesulphonyl-5-chloro-2-ethyl-7-(4-methyl-piperazin-1-yl)-pyrazolo[1,5-a]pyrimidine in 15 ml of DMF and stirred at 100° for 1 hr. After cooling to RT the reaction solution was evaporated and the residue was partitioned between 2N NaOH and CH2Cl2. The aqueous phase was extracted three times with CH2Cl2, and the combined organic phases were dried (MgSO4), filtered and evaporated. Subsequent chromatography (SiO2, CH2Cl2/MeOH/NH4OH 110:10:1) and crystallization from EtOH yielded 0.04 g (69%) of 3-benzenesulphonyl-2-ethyl-5,7-bis-(4-methyl-piperazin-1-yl)-pyrazolo[1,5-a]pyrimidine as colorless crystals, m.p. 232-235°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06194410B1 |
| Source dataset | uspto-grants-2001_02 |
| ORD ID | ord-7755ca18a3a44d5d94db102e10cd579a |
| Source note | uspto-grants-2001_02 |