HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 15700630, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 3-Formamido-3-methylamino-2-phenyl-benzo(b)thiophene | HCID 21315879 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 15700630 | HCID 15700630 | — |
Reaction Steps
34.2 g (0.13 mol) of 3-formamido-3-methylamino-2-phenyl-benzo(b)thiophene are refluxed with stirring for 4 hours with 300 milliliters of HCl at 25%. After cooling, it is diluted in water, made alkaline by sodium hydroxide solution and stirred with CH2Cl2. After the organic phase has been extracted several times 2 N NaOH 7.4 g (26% of theory) of 2-phenyl-thioindole are isolated. By evaporating the solution of CH2Cl2 dried over K2CO3, the 3-methylamino-2-phenyl-benzo(b)thiophene is obtained in the form of a crude oily product. It is dissolved in a little CHCl3 and converted into the hydrochloride by hydrochloric gas: 20.2 g (57% of theory) of colourless prisms in a mixture of ethanol and ether, decomposition from 198° C. (in a sealed tube).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04157399 |
| Source dataset | uspto-grants-1979_06 |
| ORD ID | ord-0b5baca1e11d4d3b93afeb1b3a3fbcc3 |
| Source note | uspto-grants-1979_06 |