HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 23400310, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 1-Acetoxy-2-bromoethane | HCID 13564 | — |
| Reactant | HCID 178481945 | HCID 178481945 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 23400310 | HCID 23400310 | 35.7% |
Reaction Steps
5-amino-4-(1,3-benzodioxol-5-yl)-1-methyl-1H-pyrazol-3-ol (Preparation 16) (11.39 g) was dissolved in dimethylformamide (40 mm), caesium carbonate (15.9 g) was added followed by 2-bromoethylacetate (8.16 g). The mixture was stirred at room temperature for 16 hours. The mixture was treated with water (750 ml) and extracted with ethyl acetate (2×250 ml). The organic fractions were combined washed with water (3×350 ml), brine (250 ml), dried over magnesium sulfate, filtered and evaporated. The crude product was purified on. silica (300 g) eluting with ethyl acetate:hexane (3:1) to yield the title compound as a white solid (5.57 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06610518B2 |
| Source dataset | uspto-grants-2003_08 |
| ORD ID | ord-9a18c8c753594ef6ac9d3248bad502fd |
| Source note | uspto-grants-2003_08 |