Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 2-Amino-4,6-dimethyl pyrimidine | HCID 13021 | — |
| Edukt | 2-Phenylbenzenesulfonyl isothiocyanate | HCID 13422027 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | HCID 13488534 | HCID 13488534 | 77,9% |
Reaktionsschritte
77 g of potassium N-(2-biphenylylsulfonyl)carbonimidodithioate prepared in accordance with Example 2 was suspended in 100 ml of toluene, and 37 ml of thionyl chloride was added to the suspension at 0° to 10° C. over the course of 1 hour. After the addition, the mixture was stirred at room temperature for 2 hours. The reaction mixture was filtered, and the filtrate was concentrated under reduced pressure. Distillation at reduced pressure gave 2-phenylbenzenesulfonyl isothiocyanate. On the other hand, 12.3 g of 2-amino-4,6-dimethylpyrimidine was suspended in 300 ml of dry toluene, and 27.5 g of 2-phenylbenzenesulfonyl isothiocyanate prepared as above was added. The mixture was heated under reduced pressure for 8 hours. After cooling, the resulting white precipitate was collected by filtration, and recrystallized from ethanol to give 31 g of the desired 1-(2-biphenylsulfonyl)3-(4,6-dimethylpyrimidin-2-yl)thiourea of the following formula, mp. 203°-204° C.: ##STR20##
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04559079 |
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| Quelldatensatz | uspto-grants-1985_12 |
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| ORD ID | ord-57c6e18292f84d52a6e378771ccbe330 |
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| Quellennotiz | uspto-grants-1985_12 |
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