Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 3-(4-Iodo-2-methyl-phenylamino)-isonicotinic acid hydrazide | HCID 68854415 | — |
| Reactant | C-Methylsulfanyl-methanediamine hydroiodide | HCID 86616903 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 178427893 | HCID 178427893 | 27% |
Reaction Steps
A reaction mixture of 3-(4-Iodo-2-methyl-phenylamino)-isonicotinic acid hydrazide (120 mg, 0.33 mmol, 1 eq) and C-Methylsulfanyl-methanediamine hydroiodide (104 mg, 0.47 mL, 1.45 eq) in pyridine (2 mL) in sealed tube was heated to 140° C. while stirring for 4 hrs. After cooling, it was poured into water, extracted with EtOAc, and the combined organic fractions, dried over anhydrous MgSO4. After filtration and solvent removal the remaining crude product was subjected to silica gel column chromatography (eluent:Hexane EtOAc=1:1) to afford the desired product (35 mg). [4.26 min; 393(M+1)]
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08076486B2 |
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| Source dataset | uspto-grants-2011_12 |
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| ORD ID | ord-dc361f542a62499e816501e59e002d33 |
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| Source note | uspto-grants-2011_12 |
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