HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 59410227, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | HCID 59410192 | HCID 59410192 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 59410227 | HCID 59410227 | — |
Reaction Steps
190 g (204 mmol) of the compound from Example 66A are dissolved in 1.01 l of toluene. 66.0 g (407 mmol) of 1,1′-carbonyldiimidazole are then added, and the mixture is heated at reflux for one hour. The mixture is then cooled to room temperature, and water and dichloromethane are added. The phases are separated and the organic phase is dried over sodium sulphate. After filtration, the mixture is evaporated to dryness under reduced pressure. The residue is triturated with methanol, and the solid which remains is filtered off and washed with methanol. This gives 130 g (87% of theory) of the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846934B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-01d08be58bc24c4889d9aa9341aecc20 |
| Source note | uspto-grants-2014_09 |