HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,4-Dichlorophenol → HCID 86728173, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,4-Dichlorophenol | HCID 7258 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | tert-butyl N-(3-bromopropyl)carbamate | HCID 4460490 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86728173 | HCID 86728173 | 84.8% |
Reaction Steps
To a solution of tert-butyl 3-bromopropylcarbamate (0.5 g, 2 mmol) and 3,4-dichlorophenol (0.38, 2.3 mmol) in DMF (10.5 mL) was added Cs2CO3 (1.02 g, 3.10 mmol). The reaction mixture was stirred at rt for 72 h. The reaction mixture was diluted with water and extracted with EtOAc (3×). The combined organic extracts were washed with saturated aqueous NaCl and water (1:1), dried over Na2SO4, filtered and evaporated to dryness. The crude product was purified by silica gel chromatography to provide Intermediate 3A (543 mg, 56% yield). HPLC/MS (Method B) RT=3.85 min, [M+H]+ 320.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08952180B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-38f24de0a01c46009711539946f3e130 |
| Source note | uspto-grants-2015_02 |