Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Pyridine, 2,4,6-trichloro- | HCID 27665 | — |
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 11557815 | HCID 11557815 | 26% |
Reaction Steps
A mixture of N-methyl piperazine (0.604 g, 6.04 mmol) in dry DMSO (6 mL) was prepared and NaH (0.2637 g, 10.98 mmol) was added. The resulting mixture was stirred for 30 minutes at 0° C., after which time 2,4,6-trichloropyridine (1.0 g) was added. The reaction mixture was stirred at 20 to 40° C. for 4 hours. In the reaction mixture ice cold water was added and extracted with ethyl acetate giving 3-4 times water washing. The organic layer was dried and concentrated. The residue was purified by column chromatography using 100-200 mesh silica gel. Elution of the column with 20% acetone in hexanes gave the pure product as a colorless solid. Yield: 26%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07622486B2 |
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| Source dataset | uspto-grants-2009_11 |
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| ORD ID | ord-4badc69fe51d4f93b368621f62906f0d |
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| Source note | uspto-grants-2009_11 |
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