Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethanethiol | HCID 6343 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Reactant | HCID 18988350 | HCID 18988350 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18988356 | HCID 18988356 | 55% |
Reaction Steps
500 mg (1.9 mmol) of the compound obtained in Stage B of Example 1, predissolved in 5 cm3 of methylene chloride distilled over phosphoruspentoxide are added dropwise to a mixture, cooled to 0° C., of 380 mg (2.84 mmol) of aluminum chloride and 2.3 g (37.9 mmol) of ethanethiol. After stirring for 1 h at 0° C., 1.5 eq. of aluminum chloride and 20 eq. of ethanethiol are added again. The mixture is stirred again for 1 h at 0° C. and then poured onto ice, treated with 1N hydrochloric acid and then extracted with dichloromethane. After treatment of the organic phase and purification of the crude product by chromatography on asilica column, the expected compound is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05491163 |
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| Source dataset | uspto-grants-1996_02 |
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| ORD ID | ord-460210082bfa47a2a980b0e31725cbca |
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| Source note | uspto-grants-1996_02 |
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