Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diketene | HCID 12661 | — |
| Reactant | HCID 20223068 | HCID 20223068 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 70413510 | HCID 70413510 | — |
Reaction Steps
2.7 ml of diketene was added, over 10 minutes, to a solution of 11.36 g of the compound prepared in Example 2 in 10 ml of toluene at 80° C. When the exothermic reaction was over, the reaction mixture was heated for 2 hours at 80° C. and, after cooling, it was evaporated to dryness in vacuo. The oily residue was then purified by silica gel column chromatography using ehtyl acetate containing decreasing amounts of petroleum ether as eluent. The unitary TLC fractions (chloroform:methanol 95:5 by volume) were evaporated to dryness in vacuo to give 11.61 g of the title compound as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04634712 |
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| Source dataset | uspto-grants-1987_01 |
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| ORD ID | ord-a2c2cf3b8eb94cb28aae7f189096fea9 |
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| Source note | uspto-grants-1987_01 |
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