HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium borohydride → 4,5,6,7-Tetrahydro-alpha,4,4,7,7-pentamethylbenzo[b]thiophene-methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | 1-(4,4,7,7-Tetramethyl-4,5,6,7-tetrahydro-1-benzothiophen-2-yl)ethan-1-one | HCID 23049233 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 4,5,6,7-Tetrahydro-alpha,4,4,7,7-pentamethylbenzo[b]thiophene-methanol | HCID 86740244 | 92.3% |
Reaction Steps
21.7 g of 2-acetyl-4,5,6,7-tetrahydro-4,4,7,7-tetramethylbenzo[b]thiophene are dissolved in 250 ml of ethanol and the solution is treated gradually with 5.5 g of sodium borohydride. The mixture is left to come to room temperature and is stirred for a further 2 hours. The mixture is poured on to ice, extracted with ether, the organic phase is washed once with saturated sodium chloride solution, dried and evaporated. The crude product is filtered over silica gel (eluting agent hexane/ether 3:1) and recrystallized from hexane. There are obtained 20.2 g of 4,5,6,7-tetrahydro-α,4,4,7,7-pentamethylbenzo[b]thiophene-methanol in the form of colorless crystals, m.p. 53°-55° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04659735 |
| Source dataset | uspto-grants-1987_04 |
| ORD ID | ord-962710ff8ac54ff28edddf8e76510a73 |
| Source note | uspto-grants-1987_04 |