HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl Thioglycolate → 6-Bromo-benzo[b]thiophene-2-carboxylic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl Thioglycolate | HCID 16907 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-Bromo-2-fluorobenzaldehyde | HCID 143517 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | 6-Bromo-benzo[b]thiophene-2-carboxylic acid methyl ester | HCID 22474078 | — |
Reaction Steps
Under an argon atmosphere, 1.93 g (48.3 mmol) of sodium hydride (60% in liquid paraffin) are introduced into 60 ml of absolute DMSO. At room temperature, 3.76 g (35.5 mmol) of methyl mercaptoacetate are slowly added dropwise to the reaction mixture, which is stirred at room temperature until hydrogen evolution ceases (about 15 min) A solution of 6.54 g (32.2 mmol) of 4-bromo-2-fluorobenzaldehyde and 15 ml of absolute DMSO are added at room temperature to the reaction mixture. The latter is stirred until the reaction is complete and then poured into ice-water. The resulting precipitate is filtered off with suction and dried in vacuo at 40° C. overnight. 4.06 g (46.4% of theory) of the title compound are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08772511B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-fd6073a8ada4420fb8e6807dd635ae73 |
| Source note | uspto-grants-2014_07 |