HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 85906473, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 3-Hydroxyphthalic anhydride | HCID 96580 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 85906473 | HCID 85906473 | 97.2% |
Reaction Steps
Triethylamine (0.83 g) and methanesulfonyl chloride (0.89 g) were added to a THF solution (10 mL) of 3-hydroxyphthalic anhydride (1.22 g) under ice cooling and the mixture was stirred at room temperature for 8 hours. After finishing the reaction, ether (20 mL) was added and the mixture was washed consecutively with water and saturated aqueous solution of sodium chloride and dried with anhydrous sodium sulfate. After distilling off the solvent under reduced pressure, the crude product was washed with a mixed solvent of ether and n-hexane to obtain 3-methanesulfonyloxyphthalic anhydride (1.75 g) having the melting point of 134–140° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07132455B2 |
| Source dataset | uspto-grants-2006_11 |
| ORD ID | ord-1b0eb572ad354337b809740838d237d0 |
| Source note | uspto-grants-2006_11 |