HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl bromoacetate → HCID 45486797, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl bromoacetate | HCID 7748 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 20703610 | HCID 20703610 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 45486797 | HCID 45486797 | 28.5% |
Reaction Steps
To a solution of 2-[1-(4-(N-naphth-1-yl-carbamoyl)-piperazin-2-yl)ethylamino]-4-[benzimidazol-1-yl]pyrimidine (EXAMPLE 36, Step C; 26 mg) in 0.5 mL of acetone was added potassium carbonate (11 mg) and ethyl bromoacetate (13.2 mg). The solution was stirred for 48 hours at room temperature, then diluted with 0.5 mL of water and extracted with 3×0.5 mL of CH2Cl2. The combined organics were washed with 1 mL of brine, dried with Na2SO4, and concentrated. The residue was purified by preparative HPLC (60:40 95% H2O-5% TFA:95% CH3CN-5% TFA) followed by preparative thin-layer chromatography, eluting with 95:5 25 CHCl3-isopropanol to provide 8.7 mg of the title compound. Mass spectrum (ESI) 579.3 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06316444B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-9943d8d1c2424a23ae2d0a916203acc3 |
| Source note | uspto-grants-2001_11 |