HuagongsheHuagongshe Chemistry Print Report · For research reference only
Oxetane → α-Ethyl-5-methyl-2-thiophenemethanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Oxetane | HCID 10423 | — |
| Reactant | 2-Methylthiophene | HCID 11126 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | n-Butyl lithium | HCID 61028 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | α-Ethyl-5-methyl-2-thiophenemethanol | HCID 19780497 | 17.6% |
Reaction Steps
N-Butyllithium in hexane (1.5M; 35.6 ml) was added dropwise at room temperature under nitrogen to a solution of 2-methylthiophene (5.0 g) in dry THF (50 ml). After stirring for 2.25 h, oxetane (4.42 g) in dry THF (15 ml) was added dropwise and stirring continued for 22.5 h. Saturated ammonium chloride solution (200 ml) was added and the mixture extracted with diethyl ether (3×200 ml), dried and evaporated in vacuo to give an oil. Purification by FCC on silica gel with cyclohexane-diethyl ether (1:1) as eluent gave the title compound as a pale orange oil (1.4 g). T.l.c. (cyclohexane-diethyl ether 1:1) Rf 0.31.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05002966 |
| Source dataset | uspto-grants-1991_03 |
| ORD ID | ord-94e69922e1744a8b9c6ce56a4c41268f |
| Source note | uspto-grants-1991_03 |