HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 19972646, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 19972623 | HCID 19972623 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 19972646 | HCID 19972646 | — |
Reaction Steps
A mixture of 7.52 g of 8-hydroxy-3-methyl-4-oxo-2-phenyl-4H-1-benzopyran (prepared as described in Da Re, P. et al., Ann. Chim., 1962, p.506 et seq.), 6.22 g of anhydrous potassium carbonate and 25.5 ml of 1-bromo-2-chloromethane in 70 ml of dimethylformamide was stirred at 60° C. for 25 hours. The mixture was cooled to 20°-25° C. and poured into 600 ml of water. The organic solution, obtained by extraction with dichloromethane, was washed with aqueous sodium chloride solution and dried on anhydrous sodium sulfate. The solvents and excess 1-bromo-2-chloromethane were evaporated off in vacuo to yield 8.8 g of the title compound, m.p. 141°-142° C. after crystallization from chloroform: hexane.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05605896 |
| Source dataset | uspto-grants-1997_02 |
| ORD ID | ord-011924d4768f477d898914dc1be0d370 |
| Source note | uspto-grants-1997_02 |