HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 11417330, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Phosphorus oxide (P4O10) | HCID 14812 | — |
| Reactant | 3,4,5-Trimethoxytoluene | HCID 80922 | — |
| Reactant | 3,6-Dichloro-2-methylbenzoic acid | HCID 11195073 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Methyl t-butylether hexane | HCID 21982663 | — |
| Product | HCID 11417330 | HCID 11417330 | 88.4% |
Reaction Steps
14 g (68.29 mmol) of 2,5-dichloro-6-methylbenzoic acid were introduced into 1000 ml of dichloromethane. 11.2 g (61.6 mmol) of 3,4,5-trimethoxytoluene and 28 g of finely ground phosphorus pentoxide were added. After 2 hours of stirring at room temperature, the reaction solution, which by now was orangey red, was poured into water and extracted three times with dichloromethane. The combined organic phases were washed twice with water, dried with sodium sulfate and concentrated, and the reaction product was then isolated by column chromatography using a methyl tert-butyl ether/hexane gradient. This gave 20.1 g of the title compound (yield 80%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06919485B2 |
| Source dataset | uspto-grants-2005_07 |
| ORD ID | ord-ea9a12b0c1e54f7fb59341ba4c6d11ac |
| Source note | uspto-grants-2005_07 |