HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl Ethyl Ketone → HCID 13290006, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl Ethyl Ketone | HCID 6569 | — |
| Reactant | Ethyl bromoacetate | HCID 7748 | — |
| Reactant | HCID 13290005 | HCID 13290005 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 13290006 | HCID 13290006 | 84.9% |
Reaction Steps
A mixture of 3.7 g of 6,7-dichloro-5-hydroxy-3-methylbenzo[b]thiophene, 4.3 g of ethyl bromoacetate and 20 ml of 2-butanone containing 5 ml of dimethylformamide is stirred at 60°-70° for 2 hours. The cooled mixture is diluted with ice-water and extracted 3 times with ether. The combined ether extract is dried over anhydrous magnesium sulfate and concentrated under vacuum to a brownish oil. Purification of the crude product is effected by column chromatography (alumina/ether). The purified ester is recrystallized from ether-pentane to give 4.3 g of ethyl [(6,7-dichloro-3-methylbenzo[b]thien-5-yl)oxy]acetate as fluffy needles, mp 115°-117°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04528399 |
| Source dataset | uspto-grants-1985_07 |
| ORD ID | ord-f8ae12620a63491585651e3c81e8fd90 |
| Source note | uspto-grants-1985_07 |