Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | Carbamic acid, N-(4,6-dimethoxy-2-pyrimidinyl)-, phenyl ester | HCID 10945667 | — |
| Reactant | HCID 23028111 | HCID 23028111 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 59517550 | HCID 59517550 | — |
Reaction Steps
As shown in the above reaction scheme, 2-ethyl-6-ethylthioimidazo[1,2-b]pyridazin-3-ylsulfonamide (0.19 g, 0.66 mmol) and phenyl N-(4,6-dimethoxypyrimidin-2-yl)carbamate (0.20 g, 0.73 mmol) were suspended in acetonitrile (5 ml) and stirred at room temperature, during which DBU (0.11 g, 0.73 mmol) was added thereto. After the mixture was stirred at room temperature for 2 hours, the reaction solution was poured into water (50 ml) and adjusted to pH 2 with dilute hydrochloric acid. The precipitated crystals were collected by filtration, and washed with water and ether in this order. The crystals were dried under reduced pressure to give the title compound as colorless crystals. The yield was 0.18 g (58%), and the melting point was 160 to 165° C. (dec.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07816526B2 |
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| Source dataset | uspto-grants-2010_10 |
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| ORD ID | ord-c50ebfccaab54aa5a52baf09e142c227 |
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| Source note | uspto-grants-2010_10 |
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