Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Diethyl Malonate | HCID 7761 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | HCID 53978158 | HCID 53978158 | — |
| Product | HCID 18696705 | HCID 18696705 | 87% |
Reaction Steps
To a solution of 1.53 g of sodium in 100 ml of absolute methanol was added 10 ml of diethyl malonate, and then the reaction mixture was added 12.65 g of 4-(5-chloro-2,2,4,7-tetramethylindan-6-yl)-3-buten-2-one in 50 ml of absolute methanol. After refluxing for 4 hours, the reaction mixture was evaporated under reduced pressure and then added 70 g of 10% aqueous solution of NaOH. After refluxing for 4 hours, the reaction mixture was cooled to room temperature and washed twice with diethyl ether. Concentrated hydrochloric acid was added dropwise into the boiling aqueous layers until the bubble of gas ceased and then the reaction mixture was cooled to room temperature. Solid produce was collected and dried to afford 11.9 g of the titile compound as yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06096930 |
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| Source dataset | uspto-grants-2000_08 |
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| ORD ID | ord-4e5bcfb032364682bfbe2ce502848080 |
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| Source note | uspto-grants-2000_08 |
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