HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorosulfonic acid → HCID 86655226, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorosulfonic acid | HCID 24638 | — |
| Reactant | HCID 86655224 | HCID 86655224 | — |
| Product | HCID 86655226 | HCID 86655226 | 43.1% |
Reaction Steps
Chlorosulfonic acid (5.8 g, 49 mmol) was cooled to 0° C., then 2,2,2-trifluoro-N-(3-(2-(methylsulfonyl)ethyl)phenyl)acetamide (2 g, 6.8 mmol) was added slowly. The reaction mixture was allowed to warm to room temperature. Two hours later, the reaction was poured onto ice. The aqueous layer was extracted with ethyl acetate 3 times. The combined organic phase was washed with brine, dried over sodium sulfate. The crude product was purified by pre-HPLC (column: Luna 300×50.0 mm, 10 um; liquid phase: [A-H2O+0.05% TFA; B-MeCN] B %: 0%-27%, 23 min) to give 2-(2-(methylsulfonyl)ethyl)-4-(2,2,2-trifluoroacetamido)benzenesulfonic acid (1.1 g, yield 28%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08461134B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-0e5d4b8810a74f68882a018c96cde0c7 |
| Source note | uspto-grants-2013_06 |