Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Isobutanol | HCID 6560 | — |
| Reactant | bismuth(III) bromide | HCID 82232 | — |
| Reactant | Methyl 4-(1-hydroxyethyl)benzoate | HCID 586417 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | HCID 89581006 | HCID 89581006 | 76.2% |
Reaction Steps
To a solution of 2-methylpropan-1-ol (150 mg, 2 mmol) in perchloromethane (4 mL) was added bismuth(III) bromide (900 mg, 2 mmol). The mixture was stirred at room temperature for 30 minutes then methyl 4-(1-hydroxyethyl)benzoate (180 mg, 1 mmol) was added and the mixture was stirred at room temperature for 12 hours. The suspension was concentrated in vacuum and quenched with aqueous 1N hydrochloric acid (5 mL). The residue was taken up with water (50 mL) and extracted with dichloromethane (50 mL). The combined extract was dried over sodium sulphate, evaporated and purified by column chromatography (silica gel, petroleum ether/ethyl acetate=20:1) to give the product methyl 4-(1-isobutoxyethyl)benzoate (0.18 g, 76%) as colorless oil. 1H NMR (300 MHz, CD3OD) δ 8.01 (d, J=8.1 Hz, 2H), 7.36 (d, J=8.1 Hz, 2H), 4.44-4.41 (m, 1H), 3.12-3.00 (m, 2H), 1.87-1.82 (m, 1H), 1.44 (d, J=6.3 Hz, 3H), 0.88 (d, J=6.6 Hz, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09051269B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-39288803b42c4e9e9f9749a18c093837 |
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| Source note | uspto-grants-2015_06 |
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