Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium methanolate methanol | HCID 23694274 | — |
| Reactant | HCID 86742525 | HCID 86742525 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 21285473 | HCID 21285473 | — |
Reaction Steps
A mixture comprising 2.86 g of the thiophenolate thus obtained, 30 ml of dried methanol and 3.0 ml of a 28% sodium methoxide methanol solution, was stirred at room temperature for 15 hours. Then, 1.5 ml of a 28% sodium methoxide methanol solution was added, and the mixture was stirred for further 5 hours. The reaction mixture was acidified to a pH of about 2 by gradually adding concentrated hydrochloric acid thereto, and then the solvent was distilled off. Water was poured into the dark brown oily residue thus obtained, and the mixture was extracted with benzene. The benzene layer was washed sequentially with water and a saturated sodium chloride aqueous solution, and dried over sodium sulfate. Then, the solvent was distilled off to obtain a dark brown oily substance. The oily substance was purified by silica gel column chromatograph by using benzene-n-hexane (2:1, v/v) as the developer, whereby 1.13 g of the above identified compound was obtained as a colorless oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04783462 |
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| Source dataset | uspto-grants-1988_11 |
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| ORD ID | ord-083b80dd1ce948a9893bf496b701a137 |
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| Source note | uspto-grants-1988_11 |
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