HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 12109548, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | m,alpha-Dichlorotoluene | HCID 12103 | — |
| Reactant | Acetonitrile--water (1/1) | HCID 18373917 | — |
| Reactant | 3-Piperazin-1-ylmethyl-pyrimido[5,4-e][1,2,4]triazine-5,7-diamine TFA salt | HCID 86589000 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 12109548 | HCID 12109548 | 29.2% |
Reaction Steps
To a stirred solution of 3-Piperazin-1-ylmethyl-pyrimido[5,4-e][1,2,4]triazine-5,7-diamine TFA salt 5 (50 mg; 0.08 mmol; prepared in EXAMPLE 4) in dry DMF (1.0 mL) was added m-chlorobenzyl chloride (0.015 mL; 0.12 mmol) followed by potassium carbonate (55 mg; 0.40 mmol). The mixture was allowed to stir for 24 h at room temperature then taken up into CH3CN/H2O/0.1% TFA. The mixture was purified by reverse phase HPLC (Rainin C18, 0% CH3CN to 50% CH3CN gradient, CH3CN/H2O, 0.1% TFA) and the bright yellow fractions containing the product were lyophilized after removal of CH3CN in vacuo to give 9 mg of yellow colored 3-[4-(3-Chloro-benzyl)-piperazin-1-ylmethyl]-pyrimido[5,4-e][1,2,4]triazine-5,7-diamine as the trifluoroacetate salt.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06642381B2 |
| Source dataset | uspto-grants-2003_11 |
| ORD ID | ord-bdb1f3f457564229a854df120a434e0b |
| Source note | uspto-grants-2003_11 |