HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 13290064, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Ethyl bromoacetate | HCID 7748 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 13290063 | HCID 13290063 | — |
| Solvent | Methyl Ethyl Ketone | HCID 6569 | — |
| Product | HCID 13290064 | HCID 13290064 | 85.4% |
Reaction Steps
To a mixture of 22.4 g of 6,7-dichloro-5-hydroxy-2,3-dimethylbenzo[b]thiophene is added a mixture of 18.23 g of ethyl bromoacetate in 100 ml of 2-butanone, followed by 15 g of potassium carbonate and 7.5 ml of sieve-dried dimethylformamide. The reaction mixture is stirred at 95°-100° for 21/2 hrs, allowed to cool and filtered. The filtrate is added 100 ml of water and the mixture is extracted with ethyl ether. The organic layers are separated, washed, dried over anhydrous magnesium sulfate, filtered and the solvent is removed to give a solid. The solid is recrystallized from acetone-hexane to give 25.8 g of ethyl[(6,7-dichloro-2,3-dimethylbenzo[b]thien-5-yl)oxy]acetate, mp 102°-104°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04537976 |
| Source dataset | uspto-grants-1985_08 |
| ORD ID | ord-2436d46f7d4345d58765944f71fdcaa5 |
| Source note | uspto-grants-1985_08 |