HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 69313151, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | 2-(3-Bromopropyl)-5,5-dimethyl-1,3-dioxane | HCID 3528570 | — |
| Reactant | HCID 178481684 | HCID 178481684 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 69313151 | HCID 69313151 | 65% |
Reaction Steps
4-Methyl-5-quinolin-6-yl-4H-[1,2,4]triazole-3-thiol (0.5 g, 2.07 mmol), 2-(3-Bromo-propyl)-5,5-dimethyl-[1,3]dioxane (0.49 g, 2.07 mmol) and lithium hydroxide (50 mg) were heated in dimethylformamide at 100° C. for 3 h. The mixture was cooled and partitioned between water (80 ml) and ethyl acetate (100 ml). The layers were separated and the aqueous re-extracted with ethyl acetate (100 ml). The combined organic portions were washed with brine (100 ml) and then dried (Na2SO4), filtered and evaporated to give a colourless oil. Purification by silica gel chromatography (eluent EtOAc—10% MeOH:EtOAc) which gave the title compound as a colourless solid (0.53 g, 65%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07429579B2 |
| Source dataset | uspto-grants-2008_09 |
| ORD ID | ord-06d9d6a8ad7f47798556e3ba4f535270 |
| Source note | uspto-grants-2008_09 |