HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichlorophen → 2,10-dichloro-12H-dibenzo[d,g][1,3]dioxocine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichlorophen | HCID 3037 | — |
| Reactant | Diiodomethane | HCID 6346 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2,10-dichloro-12H-dibenzo[d,g][1,3]dioxocine | HCID 14900556 | 84.1% |
Reaction Conditions
| Temperature | 105 °C |
|---|
Reaction Steps
To a solution of bis-(5-chloro-2-hydroxyphenyl)-methane (24.4 g, 90.7 mmol) in dry DMF (340 mL) was added diiodomethane (25.5 g, 95.0 mmol) and potassium carbonate (18.2 g, 132 mmol). The mixture was stirred at 105° C. for 16 h. The mixture was added to ice water (1200 mL) and stirred for 30 min. The product was isolated by filtration, and washed with water and suspended in a mixture of ethanol (200 mL) and 4N NaOH (50 mL). The mixture was heated at 80° C. for 1 h. The mixture was added to water (600 mL) and 21.45 g (84%) 2,10-dichloro-12H-dibenzo[d,g][1,3]-dioxocin was isolated by filtration.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06723731B2 |
| Source dataset | uspto-grants-2004_04 |
| ORD ID | ord-68571ba914494e319af7ee49a194dc8d |
| Source note | uspto-grants-2004_04 |