HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 13290078, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Ethyl bromoacetate | HCID 7748 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 13290077 | HCID 13290077 | — |
| Solvent | Methyl Ethyl Ketone | HCID 6569 | — |
| Product | HCID 13290078 | HCID 13290078 | 91.4% |
Reaction Steps
To a mixture of 10 g of 6,7-dichloro-5-hydroxy-2-isobutylbenzo[b]thiophene and 200 ml 2-butanone is added a mixture of 6.9 g of ethyl bromoacetate in 50 ml of 2-butanone and by 6.6 g of potassium carbonate and 3.4 ml sieve-dried dimethylformamide. The reaction mixture is stirred at 95°-100° for 2 hrs, allowed to cool and filtered. To the filtrate is added 100 ml of water and 100 ml of ether. The organic layers are combined, washed, dried over anhydrous magnesium sulfate, filtered and the solvent is removed to give a solid. Recrystallization from ethyl ether and hexane gives 12 g of ethyl[(6,7-dichloro-2-isobutylbenzo[b]-thien-5-yl)oxy]acetate, mp 75°-76°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04528399 |
| Source dataset | uspto-grants-1985_07 |
| ORD ID | ord-8d2f5a156d58433faec56b55643ff27e |
| Source note | uspto-grants-1985_07 |