Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 15709970 | HCID 15709970 | — |
| Reactant | Boron tribromide dichloromethane | HCID 22277759 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 20316583 | HCID 20316583 | — |
Reaction Steps
Into a 100 ml flask equipped for stirring, under a nitrogen atmosphere are placed 0.55g of 6-dimethylamino-4-(4-methoxyphenyl)-4-phenyl-heptane-3-one, 40 ml of methylene chloride and 12.1 ml of a solution of boron tribromide/methylene chloride (10% solution obtained commercially). The mixture was allowed to stir at room temperature overnight. Thereafter, 30 ml. of methanol was added with cooling. The residual oil, obtained upon removing the solvent at reduced pressure, was treated with 7 ml of water, whereupon the crude product crystallized. After filtration and washing with water, the solid was recrystallized from water to give 0.137 g of the above captioned product m.p. 246°-247.5° C. Concentration of the aqueous filtrate yielded a small second crop of 20 mg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04104367 |
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| Source dataset | uspto-grants-1978_08 |
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| ORD ID | ord-0876d7848ec0408bbd0d6c8412ad4e69 |
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| Source note | uspto-grants-1978_08 |
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