Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cumene | HCID 7406 | — |
| Reactant | 4-Chlorobutyryl chloride | HCID 78370 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-Chloro-4'-isopropylbutyrophenone | HCID 98744 | 86.9% |
Reaction Steps
Slurry aluminum chloride (140.9 g, 1.075 mol) and 4-chlorobutyryl chloride (148 g, 1.05 mol) in methylene chloride (1.0 L) add, by dropwise addition, cumene (125 g, 1.04 mol) over a thirty minute period under a nitrogen atmosphere while maintaining the internal temperature between 5-8° C. with an ice bath. Allow the stirred solution to come to room temperature and continue stirring under nitrogen for 14 hours. Cautiously add the methylene chloride solution to 1 L of crushed ice with stirring and add additional methylene chloride (400 mL). Separate the organic phase and wash with 10% hydrochloric acid (3×300 mL), water (3×300 mL), 10% sodium bicarbonate (3×300 mL) and water (3×300 mL). Dry (MgSO4), filter and wash with methylene chloride (150 mL). Evaporate the solvent to give the title compound (203 g, 86%) as a clear oil which crystallizes on standing; mp 35-37° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06479663B2 |
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| Source dataset | uspto-grants-2002_11 |
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| ORD ID | ord-495de7ed011943d9bae265d47a365af3 |
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| Source note | uspto-grants-2002_11 |
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