HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon tetrabromide → HCID 117687689, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon tetrabromide | HCID 11205 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Ethanol, 2-[2-[2-(triphenylmethoxy)ethoxy]ethoxy]- | HCID 11825346 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 117687689 | HCID 117687689 | — |
Reaction Steps
A solution of carbon tetrabromide (8.3 g, 25 mmol) and 10 g of 2-[2-(2-triphenylmethoxyethoxy)ethoxy]ethanol are stirred together in 75 mL dichloromethane at 0° C. To this solution is added a solution of 6.7 g triphenylphosphine (25 mmol) in 75 mL dichloromethane dropwise over 1½ hours at 0° C. After stirring for an additional 2 hours, the solution is evaporated to dryness and the residual solids are resuspended in 150 mL diethyl ether. The triphenylphosphine by-product is removed via vacuum filtration and the product is then purified via column chromatography over silica gel, eluting with dichloromethane.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09273074B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-04bd209d2dc448ee814eb1632401324a |
| Source note | uspto-grants-2016_03 |