HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 117926708, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1,2-Dibromoethane | HCID 7839 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 2-Bromo-5-hydroxypyridine | HCID 2762865 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 117926708 | HCID 117926708 | 86% |
Reaction Steps
6-Bromo-3-hydroxypyridine (2 g, 11.56 mmol) was dissolved in anhydrous DMF (20 mL); to which 1,2-dibromoethane (10 g, 57.82 mmol) was added and the reaction mixture was stirred at room temperature for 16 h. After completion of the reaction, water (100 mL) was added to it and extraction was carried out using EtOAc (30 mL×3). The combined organic layers were washed with water (100 mL), brine (100 mL), dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The residue was purified using silica gel column chromatography to provide Q-1-I (2.7 g, 86% yield). LCMS: m/z; 280.0 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09233983B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-a5367032fa624ee19cd5a4d5d5e5f3b9 |
| Source note | uspto-grants-2016_01 |