Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Carbon Disulfide | HCID 6348 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 6-Chloro-4-(isopropylamino)nicotinohydrazide | HCID 89689668 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178456766 | HCID 178456766 | — |
Reaction Steps
6-chloro-4-(isopropylamino)nicotinohydrazide (10) (1.5 g, 8.7 mmol) was taken in EtOH (10 mL): H2O (5 mL). Added KOH (13 mmol, 1.5 equiv.) followed by the addition of CS2 (87 mmol, 10 equiv.) to the reaction mixture and heated at 90° C., overnight. The reaction mass was concentrated under reduced pressure to remove solvents from the reaction mixture. The crude material obtained was taken to next step as such without purification. LC/MS: Purospher@star RP-18, 4×55 mm, 3 μm; Solvent A=10% ACN: 90% H2O: 20 mM NH4OAc; Solvent B=90% ACN: 10% H2O: 20 mM NH4COOAc; gradient 0-100% B over 1.5 min (3.2 min run time); retention time: 1.27 min; LCMS (ES-API), m/z 269.0 (M−H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09242975B2 |
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| Source dataset | uspto-grants-2016_01 |
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| ORD ID | ord-fde6a55566924b978a98d227d580bf38 |
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| Source note | uspto-grants-2016_01 |
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