HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 23114095, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 23113966 | HCID 23113966 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 23114095 | HCID 23114095 | 99% |
Reaction Steps
To a mixture of 3-(4-isopropylphenyl)-4,6,7-trimethyl-2,3-dihydro-1-benzofuran synthesized in Reference Example 13 (6.10 g, 21.8 mmol) and sodium acetate (1.97 g, 24.0 mmol) in acetonitrile (30 mL) was added bromine (1.17 mL, 22.9 mmol), and the mixture was stirred at the same temperature for 1 hour. Water was poured into the reaction mixture, which was extracted with ethyl acetate. The extract was washed with a saturated sodium hydrogen carbonate solution and water, dried over magnesium sulfate, filtered and then concentrated under reduced pressure. The obtained residue was crystallized from methanol to obtain 7.90 g (yield 99%) of the title compound. Melting point: 86-87° C. (methanol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07507841B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-0ed47b445b744e1f84ecf4da64e12ce0 |
| Source note | uspto-grants-2009_03 |