Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 18186818 | HCID 18186818 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 18186921 | HCID 18186921 | — |
Reaction Steps
A mixture of the product from step 1 above (1.04 g, 5.29 mmol), piperazine (1.32 g, 15.3 mmol), and K2CO3 (0.81 g, 5.82 mmol) in acetonitrile (6 mL) was heated in a sealed pyrex flask at 85° C. for 8.5 h. The reaction mixture was diluted with dichloromethane, filtered, and concentrated in vacuo. The semi-solid residue was purified by column chromatography on silica gel (18×5 cm) using CHCl3/MeOH (9:1) as eluent to furnish an oil. This material was redissolved in ethyl acetate, filtered, and concentrated in vacuo. This gave 0.98 g (75%) of the title compound as a yellow sticky oil. HRMS m/z calcd for C12H14N4S (M)+ 246.0939, found 246.0943. Anal. (C12H14N4S) C, H, N.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06593330B2 |
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| Source dataset | uspto-grants-2003_07 |
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| ORD ID | ord-76f40c2864f24a918c67f569d0fb50a8 |
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| Source note | uspto-grants-2003_07 |
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