Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methyl isothiocyanate | HCID 11167 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Thiourea | HCID 2723790 | — |
| Reactant | HCID 178513172 | HCID 178513172 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 10539891 | HCID 10539891 | 29% |
Reaction Steps
The synthesis method of Example 1-(2) was applied. The compound (5.4 g) obtained in (1) above and dimethylsulfoxide (50 ml) were used as reagents and the mixture was stirred at 180° C. for 1 hour. After the reaction, the reaction mixture was ice-cooled and used as it was in the next reaction. The conversion to a thiourea compound was performed according to the method of Example 7-(3). The above-mentioned solution, a 1N aqueous sodium hydroxide solution (20 ml) and methyl isothiocyanate (1.5 g) were used as reagents. After the reaction, the mixture was neutralized with 3N hydrochloric acid and the resulting powder was collected by filtration. The powder was subjected to silica gel column chromatography (chloroform) and recrystallization (chloroform) to give 2.9 g of white crystals (yield 29%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05750545 |
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| Source dataset | uspto-grants-1998_05 |
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| ORD ID | ord-6052e63cbc9b4988bd62b48c4e0631c4 |
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| Source note | uspto-grants-1998_05 |
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