HuagongsheHuagongshe Chemistry Print Report · For research reference only
Oxonium, triethyl-, hexafluorophosphate(1-) (1:1) → HCID 9998689, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Oxonium, triethyl-, hexafluorophosphate(1-) (1:1) | HCID 167684 | — |
| Reactant | HCID 22595112 | HCID 22595112 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 9998689 | HCID 9998689 | 69% |
Reaction Steps
2,4-Dibenzyloxybenzoic acid was reacted with oxalyl chloride in toluene and DMF at 0-25° C. to give an acid chloride. The acid chloride was reacted with aqueous ammonia in methylene chloride to yield 87% (over 2 steps) of 2,4-dibenzyloxybenzamide. 2,4-Dibenzyloxybenzamide was reacted with triethyloxonium hexafluorophosphate in methylene chloride to yield 69% of ethyl 2,4-dibenzyloxybenzimidate. The ethyl 2,4-dibenzyloxybenzimidate was hydrogenated over a palladium/carbon catalyst with 1 atmosphere of hydrogen gas in ethanol, to yield 75% of ethyl 2,4-dihydroxybenzimidate. The overall yield for the reaction sequence was 34% for six steps.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06846958B2 |
| Source dataset | uspto-grants-2005_01 |
| ORD ID | ord-9f8ac02056c343ac9b325bb631ba5512 |
| Source note | uspto-grants-2005_01 |