HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 10741054, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Chlorosulfonic acid | HCID 24638 | — |
| Reactant | 2-(4-Fluorophenyl)-3-(4-methylsulfonylphenyl)thiophene | HCID 10336873 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 10741054 | HCID 10741054 | — |
Reaction Steps
2-(4-Fluorophenyl)-3-[4-(methylsulfonyl)phenyl]thiophene (1.1 g) was added portionwise to chlorosulfonic acid (1 ml), and the mixture was stirred at ambient temperature for 1 hour. The mixture was added to a mixture of 25% methylamine aqueous solution (20 ml) and tetrahydrofuran (20 ml), and stirred at 0° C. for 1 hour. The reaction mixture was extracted with ethyl acetate, and the extract was washed with water, dried and concentrated. The oily residue (2.4 g) was purified by column chromatography on silica gel eluting with a mixture of chloroform and methanol (20:1), and then recrystallized from ethanol to give colorless crystals of N-methyl-5-(4-fluorophenyl)-4-[4-(methylsulfonyl)phenyl]thiophene-2-sulfonamide (1.1 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05571810 |
| Source dataset | uspto-grants-1996_11 |
| ORD ID | ord-34c7054137cd481cb214312f6f65e969 |
| Source note | uspto-grants-1996_11 |