Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Hexafluoroacetone trihydrate | HCID 36719 | — |
| Reactant | HCID 29790482 | HCID 29790482 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 86591940 | HCID 86591940 | — |
Reaction Steps
Molecular sieves powder (4A) (1 g) was added to a mixture of crude intermediate N-(pyridin-4ylmethyl)-1,3-thiazol-2-amine prepared above (2.5 g 13 mmol) and hexafluoroacetone trihydrate (4 g, 18.1 mmol) in benzene (3 ml). The mixture was heated at 80° C. for 24 h. Acetonitrile was added and mixture was filtered. Solvent was evaporated under reduced pressure. The residue was chromatographed on silica gel, eluting with a 95:5 mixture of CHCl3 and CH3OH, to afford the title compound as an orange solid (1.1 g). 1H NMR (DMSO-d6) δ 4.3 (d, 2H), 7.10 (s, 1H), 7.42 (d, 2H); 7.78 (d, 2H), 8.45 (brs, 1H), 8.82 (brs, 1H); ESIMS: m/z 356 (M−H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07524969B2 |
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| Source dataset | uspto-grants-2009_04 |
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| ORD ID | ord-2505096012264699b361f53735ded911 |
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| Source note | uspto-grants-2009_04 |
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