HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86654325, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,3-Dibromo-5-fluoro-2-methoxy-4-nitrobenzene | HCID 22504669 | — |
| Reactant | Tin dichloride dihydrate | HCID 43835034 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86654325 | HCID 86654325 | 100% |
Reaction Steps
To the solution of 8-4 (234.2 g, 0.784 mol) and concentrated HCl (720 mL) in ethanol (2.2 L) at room temperature, SnCl2.H2O (415 g, 2.0 mol) was added by portions. The mixture was stirred for 16 h. TLC showed the reaction was completed. The volatiles were removed in vacuo. The residue was quenched with cooled water (500 mL) and ethyl acetate (1.5 L). The aqueous layer was neutralized with KOH until PH=6˜7. The white precipitate was filtered off to get a clear solution, which was extracted with ethyl acetate (600 mL×3). The combined organic layers were washed with brine twice, dried over anhydrous sodium sulfate. After filtration and evaporation, 8-5 (212.7 g, 100%) was obtained as brownish white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08912220B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-a391756ec1f948629150018549acdcc5 |
| Source note | uspto-grants-2014_12 |