HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methylpiperazine → HCID 21254935, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | HCID 21254940 | HCID 21254940 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21254935 | HCID 21254935 | 50% |
Reaction Steps
0.33 ml (3 mmol) of 1-methyl-piperazine was added to a solution of 0.4 g (1.2 mmol) of 3-benzenesulphonyl-5-chloro-2-ethyl-pyrazolo[1,5-a]pyrimidin-7-ylamine in 5 ml of DMF and stirred at 90° for 1 hr. The reaction solution was evaporated and the residue was partitioned between H2O and CH2Cl2. The aqueous phase was extracted three times with 50 ml of CH2Cl2. The combined organic phases were dried (MgSO4), filtered and evaporated. Subsequent chromatography (silica gel, CH2Cl2/MeOH 9:1) and crystallization from EtOH yielded 0.24 g (50%) of 3-benzenesulphonyl-2-ethyl-5-(4-methyl-piperazin-1-yl)-pyrazolo[1,5-a]pyrimidin-7-yl-amine as colorless crystals, m.p.>250°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06194410B1 |
| Source dataset | uspto-grants-2001_02 |
| ORD ID | ord-de9bfa08e0144e49a5df9fd9e5c3efda |
| Source note | uspto-grants-2001_02 |