Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 10537603 | HCID 10537603 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 10495279 | HCID 10495279 | 67.1% |
Reaction Steps
4-Formylamino-2,3,5-trimethyl-6-(2-methyl-2-propenyl)phenol (50 g, 0.21 mol) and sodium acetate (30.5 g, 0.37 mol) were added to acetic acid (500 ml). Bromine (16.5 ml, 0.21 mol) was added dropwise to the mixture with stirring. After the reaction mixture was stirred for 30 minutes, the mixture was poured into ice water and the product was extracted with ethyl acetate. The extract was washed with aqueous saturated sodium bicarbonate solution, dried and then concentrated. The residue was dissolved in ethyl acetate again and insoluble materials were filtered off. The filtrate was concentrated and isopropyl ether was added to the residue. The crystals precipitated were filtered off to obtain the desired compound (44.0 g, yield: 65.7%), m.p. 157°-158° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05770772 |
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| Source dataset | uspto-grants-1998_06 |
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| ORD ID | ord-795b11f97c4142b3bdfa926a7ff14252 |
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| Source note | uspto-grants-1998_06 |
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