HuagongsheHuagongshe Chemistry Print Report · For research reference only
Butyl iodide → 5-Butyl-N-tert-butylthiophene-2-sulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Butyl iodide | HCID 10962 | — |
| Reactant | N-(Tert-butyl)-2-thiophenesulfonamide | HCID 765814 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 5-Butyl-N-tert-butylthiophene-2-sulfonamide | HCID 11993904 | 46% |
Reaction Conditions
| Temperature | -78 °C |
|---|
Reaction Steps
N-tert-Butylthiophene-2-sulfonamide (5 g, 0.0228 mol, see Example 1(a) above) was dissolved in THF (43 mL) under N2 and then cooled to −78° C. n-BuLi (1.6 M, 38.5 mL, 0.062 mol) was added via a syringe. The reaction mixture was stirred at −78° C. for 30 min and then at −40° C. for 2 h. Iodo-butane (5.19 mL, 0.046 mol) was added dropwise to the reaction mixture. The reaction mixture was stirred overnight at room temperature, quenched with NH4Cl (aq) and extracted with EtOAc. The combined organic phase was washed with brine, dried and concentrated in vacuo. The crude product was purified on column chromatography (Hex:EtOAc 10:1) to give the sub-title compound in 46% yield (2.92 g, 0.011 mol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07652054B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-17451990ff4a4e2f8771fd9aa96efa86 |
| Source note | uspto-grants-2010_01 |