Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Isobutyryl chloride | HCID 62325 | — |
| Reactant | 5,5,8,8-Tetramethyl-5,6,7,8-tetrahydronaphthalen-2-ol | HCID 268786 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 45272516 | HCID 45272516 | — |
Reaction Steps
The synthesis process is as set forth in the chemical reaction formula below. To 5,6,7,8-tetrahydro-2-hydroxy-5,5,8,8-tetramethylnaphthalene (204 mg, 1.00 mol) were added anhydrous dichloromethane (1 mL), aluminum chloride (148 mg, 1.12 mmol), and isobutyryl chloride (117 mg, 1.10 mmol) followed by stirring at 60° C. for 2 hours. The reaction solution was poured into cold water, and extracted by ethyl acetate. The organic layer was washed by water, a saturated sodium hydrogen carbonate aq. solution, and a saturated saline solution, dried over magnesium sulfate, and concentrated under reduced pressure. The crude product was purified by silica gel chromatography using hexane/ethyl acetate (20/1) as an elution solvent. The yield was 128 mg (47%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08765719B2 |
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| Source dataset | uspto-grants-2014_07 |
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| ORD ID | ord-0f079842e0b64a66b991d43889d3e631 |
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| Source note | uspto-grants-2014_07 |
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