HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,6-Dichloropyrazine → HCID 21906088, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,6-Dichloropyrazine | HCID 78504 | — |
| Reactant | Tert-butyl 4-hydroxypiperidine-1-carboxylate | HCID 643502 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 21906088 | HCID 21906088 | 90.1% |
Reaction Steps
A mixture of 2,6-dichloropyrazine (5.00 g, 33.6 mmol), tert-butyl 4-hydroxy-1-piperidinecarboxylate (6.76 g, 33.6 mmol) and K-t-BuO (1 M in tert-butanol; 35 mL, 35 mmol) in Et3N (200 mL) was stirred at room temperature for 12 h. The reaction was quenched with water (50 mL) and concentrated in vacuo. The residue was dissolved in ethyl acetate, washed with saturated aqueous KH2PO4, dried (MgSO4), and concentrated in vacuo. The residue was recrystallized from ethanol/water to give 9.50 g (90%) of the title compound as a white solid: mp 86-87° C.; MS m/z 313 (M)+. Anal. (C14H20ClN3O3C, H, N.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06593330B2 |
| Source dataset | uspto-grants-2003_07 |
| ORD ID | ord-60a60ffbfd6d4a24b90bb9fb7079408c |
| Source note | uspto-grants-2003_07 |