HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 67342990, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 4-Amino-1-Boc-piperidine | HCID 1268291 | — |
| Reactant | HCID 19791860 | HCID 19791860 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 67342990 | HCID 67342990 | 74% |
Reaction Steps
To a mixture of 5-chloro-3-methylpyridazine (1.3 g, 10.1 mmol) and Boc-4-aminopiperidine (2.63 g, 13.1 mmol) in NMP (13 mL) was added DIPEA (2.47 mL, 14.2 mmol). Argon was bubbled through the cloudy solution for 5 minutes before the reaction mixture was heated in the microwave for 30 minutes to 150° C. The mixture was then poured into water and extracted with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and evaporated. Purification by chromatography (silica gel, 50 g, 50 to 100% ethyl acetate in heptane) afforded the title compound (2.18 g, 74%) as an off white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08486967B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-b87a0c2eb5ff4d4f9adaffb878d0364e |
| Source note | uspto-grants-2013_07 |