HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoromethanesulfonic anhydride → HCID 89350907, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 71185803 | HCID 71185803 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 89350907 | HCID 89350907 | 47% |
Reaction Steps
To a mixture of 8-chloro-4-methoxy-1-naphthoic acid (step-6 intermediate) (0.14 g, 0.561 mmol) in DCM (5 mL) was added, DIPEA (0.20 mL, 1.12 mmol) at 0° C. After 5 min stirring, Tf2O (0.11 mL, 0.67 mmol) was added to it. The resulting mixture was stirred for 2 h before quenching with ice water. The aqueous layer was extracted with DCM, and the combined organic layer was washed with, water, brine, dried over Na2SO4 and filtered. The solvent was removed under reduced pressure and the residue was purified by column chromatography to furnish the desired trifliate intermediate as a pale yellow oil (100 mg, 47%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09006442B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-c1cf468b6ce447bebd7c23c3d985c27e |
| Source note | uspto-grants-2015_04 |