HuagongsheHuagongshe Chemistry Print Report · For research reference only
Isobutanol → 4-Isobutoxy-benzo[b]thiophene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Isobutanol | HCID 6560 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Benzo(b)thiophen-4-ol | HCID 19217 | — |
| Reactant | Diethyl azodicarboxylate | HCID 5462977 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 4-Isobutoxy-benzo[b]thiophene | HCID 59600224 | — |
Reaction Steps
Benzo[b]thiophen-4-ol (200, 4.3 g, 28.9 mmol) and iso-butanol (3.2 ml, 34.7 mmol) are dissolved under argon in 150 ml of toluene. After addition of triphenylphosphine (9.1 g, 34.7 mmol) and a 40% solution of DEAD in toluene (16.8 ml, 34.7 mmol), the mixture is stirred at 120° C. over night. After cooling down, the reaction mixture is subsequently washed with saturated aqueous NaHCO3 solution and NaCl solution, dried over Na2SO4 and evaporated under reduced pressure. Triphenylphosphinoxid is removed by crystallization from ethyl acetate and hexane and the crude product is further purified by flash chromatography (silica gel, hexane/ethyl acetate 9:1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07858781B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-b93b957aa88444a98fbd05253c086a8a |
| Source note | uspto-grants-2010_12 |