Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrazine | HCID 9321 | — |
| Reactant | HCID 86653539 | HCID 86653539 | — |
| Solvent | Diglyme | HCID 8150 | — |
| Product | HCID 58268931 | HCID 58268931 | — |
Reaction Steps
2-(6-Chloro-2-(methylthio)pyrimidin-4-yl)malononitrile (2b) (500 mg, 2.23 mmoles) was dissolved in 15 mL of diethylene glycol dimethyl ether along with of hydrazine [68.4 μL, 69.8 mg; 2.18 mmoles) and the reaction mixture sealed in a microwave vessel. The reaction was heated at 150° C. for 10 minutes (300 Watt) and then allowed to cool down. The solvent was removed under reduced pressure and the crude suspended in acetone, warmed to almost reflux and stirred. Then continued stirring while allowing to cool down to rt. The precipitate was isolated via suction filtration and washed with more acetone and air-dried. The product (3b) was obtained as a mustard colored powder (240 mg, 42% yield) and was used in the next step without further purification. LC/MS (M+1) 257, 259.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08937064B2 |
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| Source dataset | uspto-grants-2015_01 |
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| ORD ID | ord-d1bac952b7fe405dadf6b7687df8002b |
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| Source note | uspto-grants-2015_01 |
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