HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Hydroxide → HCID 67219804, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | 5-Methyl-4-nitrothiophene-2-sulfonyl chloride | HCID 21498964 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67219804 | HCID 67219804 | 82% |
Reaction Steps
To a stirred solution of 5-methyl-4-nitrothiophene-2-sulfonyl chloride [CAS No. 61714-77-0] (1.0 g, 4.14 mmol) in THF (20 ml) was added at 0° C. (ice water bath) ammonium hydroxide solution (25%, 5 ml). The reaction mixture was stirred at room temperature for 1 h, evaporated, poured into water (30 ml) and extracted with ethyl acetate (2×50 ml). The combined organic layers were washed with brine (2×30 ml), dried (MgSO4) and evaporated. The crude product was further purified by crystallization from ethyl acetate/hexane to yield 5-methyl-4-nitro-thiophene-2-sulfonamide (0.75 g, 82%) as a brown solid. MS (ISP) 221.0 [(M−H)−], mp 120° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07361659B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-069a2ee9b8ae4ad6b600927f921ef115 |
| Source note | uspto-grants-2008_04 |