HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 87491517, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| Reactant | HCID 68547613 | HCID 68547613 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 87491517 | HCID 87491517 | 69% |
Reaction Steps
6-chloro-2-hydroxy-benzo[b]thiophene-3-carboxylic acid methyl ester (2.46 g, 10.1 mmol) was cooled to 0° C. in a solution of DCM (25 ml) and Et3N (25 ml). Tf2O (2.56 ml, 15.2 mmol, 1.5 equiv) was added dropwise, then stirred for 1 hr. The resulting solution was washed twice with water, saturated NaHCO3, then water, followed by drying over MgSO4. This was filtered and the solvent removed in vacuo. The crude material was purified by column chromatography leaving 2.61 g (68%) of 6-chloro-2-trifluoromethanesulfonyloxy-benzo[b]thiophene-3-carboxylic acid methyl ester as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07674822B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-620bc8c58c444e858f82418d4f28dae7 |
| Source note | uspto-grants-2010_03 |