HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 67294316, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 67300315 | HCID 67300315 | — |
| Solvent | Trifluoroacetic anhydride | HCID 9845 | — |
| Product | HCID 67294316 | HCID 67294316 | — |
Reaction Steps
5.5 g of 5-(4-fluorobenzoyl)-2,2,8-trimethyl-4H-[1,3]dioxino[4,5-c]pyridine 7-oxide was dissolved in 20 mL dichloromethane (DCM) in 5 mL of Trifluoroacetic anhydride (TFAA) followed by vigorous boiling. When the boiling subsided an additional 30 mL of TFAA was added and the solution was stirred overnight (14 h). TLC revealed completion of the reaction (Rf EtOAc; (s.m. 0.2), product 0.9). The DCM was removed by evaporation and the solvent switched to MeOH (100 mL). This solution was stirred for 30 min after which evaporation affording thick oil. Toluene was added and removed under high vacuum yielding a foam containing the desired product (1d).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08283366B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-156e6b1505a7473db46383111fe0ba3c |
| Source note | uspto-grants-2012_10 |