Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | 1,1'-(Diazomethylene)bis(benzene) | HCID 61230 | — |
| Reactant | HCID 57234141 | HCID 57234141 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18516692 | HCID 18516692 | 22.7% |
Reaction Steps
55 g of 4-hydroxy-8-methyl-7-(tetrahydro-2H-pyran-2-yl)-2H-1-benzopyran-2-one is introduced into 250 ml of anhydrous dimethylformamide heated to 40° C., and a solution of 58.3 g of diphenyldiazomethane in 250 ml of DMF is added dropwise. The addition is made over 3 hours while maintaining the temperature at 40° C. Several portions of 3 g of diphenyldiazomethane are added again and agitation is carried out for one hour at 40° C. The reaction medium is poured into 2 l of sulphuric ether. The organic solution is washed with an aqueous solution of sodium bicarbonate, with a solution of soda (0.1 M), with water and with salt water followed by evaporation to dryness. The residue is agitated in an isopropyl ether-hexane mixture (1-2) followed by separation. The insoluble part is dried. 20.5 g of sought product is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06579902B1 |
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| Source dataset | uspto-grants-2003_06 |
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| ORD ID | ord-e7640aaed784442ab4aff0e2aac8e699 |
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| Source note | uspto-grants-2003_06 |
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