HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 18399625, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 18399619 | HCID 18399619 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 18399625 | HCID 18399625 | 29% |
Reaction Steps
A solution of 0.70 mL of bromine in 3.45 mL of acetic acid was added dropwise over a period of 60 minutes to a solution of 3.56 g of Compound 3A in 34.5 ml, of acetic acid at 20-25° C. while stirring. After stirring further for 2.5 hours at 20-25° C., the mixture was poured into ice water and extracted with diethyl ether (2×80 mL). The combined organic layers were washed with water (2×80 ml), 10% aqueous sodium carbonate (100 mL) and water (3×80 mL), dried over sodium sulphate and evaporated to dryness in vacuo. The crude product was purified by flash chromatography in n-hexane/chloroform (6:4) to yield 1.31 g (29%) of Compound 3B.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06486163B1 |
| Source dataset | uspto-grants-2002_11 |
| ORD ID | ord-baa44cc1cd204ea6a4a0facf7e8bcd9f |
| Source note | uspto-grants-2002_11 |