HuagongsheHuagongshe Chemistry Print Report · For research reference only
Morpholine → HCID 58547921, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Morpholine | HCID 8083 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Reactant | HCID 58547976 | HCID 58547976 | — |
| Catalyst | Binap, (A+-)- | HCID 634876 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Product | HCID 58547921 | HCID 58547921 | 77.7% |
Reaction Steps
To a solution of tert-butyl 4-((3-bromopyridin-2-yl)oxy)piperidine-1-carboxylate (see PREPARATION P20.4; 4 g, 11.2 mmol), morpholine (1.46 g, 16.8 mmol), Pd2(dba)3 (513 mg, 0.56 mmol), 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (BINAP) (349 mg, 0.56 mmol), sodium tert-butoxide (t-BuONa) (2.15 g, 22.4 mmol) then the reaction mixture was stirred at 90° C. for overnight. The mixture was left to reach room temperature, then the reaction mixture was filtered through a pad of CELITE® and the filter cake was washed with CH2Cl2 (3×20 mL). The combined filtrates were evaporated in vacuo and the residue was purified by column chromatography to give the product (3.1 g, 8.7 mmol, yield 70%). ESI-MS (M+1): 364 calc. for C19H29N3O4 363.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08497265B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-eca7af5c3fe04d46adef2f3909e22bfe |
| Source note | uspto-grants-2013_07 |