HuagongsheHuagongshe Chemistry Print Report · For research reference only
Morpholine → 4-Morpholinobenzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Morpholine | HCID 8083 | — |
| Reactant | 4-Chlorobenzonitrile | HCID 12163 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | 4-Morpholinobenzonitrile | HCID 394808 | 96.7% |
Reaction Steps
An oven-dried resealable Schlenk tube was purged with argon and charged with Pd2(dba)3 (11.5 mg, 0.025 mmol, 5 mol % Pd), 2 [Example 1] (14.8 mg, 0.075 mmol, 7.5 mol %), NaOt-Bu (68 mg, 0.71 mmol) and 4-chlorobenzonitrile (69 mg, 0.50 mmol). The tube was purged with argon then DME (0.5 mL) and morpholine (53 μL, 0.61 mmol) were added through a rubber septum. The septum was removed, the tube was sealed with a teflon screw cap and the mixture was stirred at room temperature for 26 h. The reaction was then diluted with EtOAc (20 mL), filtered through celite and concentrated in vacuo. The crude material was purified by flash chromatography on silica gel to afford 91 mg (96%) of a tan solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06307087B1 |
| Source dataset | uspto-grants-2001_10 |
| ORD ID | ord-b25ff1d8a2334671ab7698d2f783a758 |
| Source note | uspto-grants-2001_10 |