HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 86619567, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1-Bromo-4-chlorobutane | HCID 81364 | — |
| Reactant | HCID 86619566 | HCID 86619566 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86619567 | HCID 86619567 | 98.6% |
Reaction Steps
Sodium hydride (0.55 g) is added at room temperature to a solution of 5-bromo-3-(2-chloro-phenyl)-pyrazin-2-ylamine (0.23 g) in DMF (10 mL). Subsequently 1-bromo-4-chlorobutane (0.21 g) is added and the mixture is stirred for 3 h. Citric acid (10%, 20 mL) is added and the mixture is extracted with ethyl acetate (3×50 mL). Organic phases were pooled, washed with sodium bicarbonate and brine, dried with Na2SO4 and the solvent was evaporated. The residue was purified by chromatography on silica gel with heptane/ethyl acetate 2:1 to yield 0.27 g of the title compound as a yellow oil, MS (ISP) 338.1, 340.0 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07812028B2 |
| Source dataset | uspto-grants-2010_10 |
| ORD ID | ord-0ba7f0d964cb4124b7ceb117377d9f35 |
| Source note | uspto-grants-2010_10 |