HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → 4-[1-Phenyl-1-(5-(1-methylazetidin-3-yl)-1,3,4-oxadiazol-2-yl)methylene]piperidine-1-carboxylic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | 4-[1-Phenyl-1-(5-(azetidin-3-yl)-1,3,4-oxadiazol-2-yl)methylene]piperidine-1-carboxylic acid tert-butyl ester | HCID 67046441 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 4-[1-Phenyl-1-(5-(1-methylazetidin-3-yl)-1,3,4-oxadiazol-2-yl)methylene]piperidine-1-carboxylic acid tert-butyl ester | HCID 67046424 | 39.5% |
Reaction Steps
To a solution of 4-[1-phenyl-1-(5-(azetidin-3-yl)-1,3,4-oxadiazol-2-yl)methylene]piperidine-1-carboxylic acid tert-butyl ester (0.029 g, 0.074 mmol) in MeOH (5 mL) was added formaldehyde (0.322 mL, 57% solution in H2O) dropwise at rt. A solution of NaCNBH3 (0.026 g, 0.415 mmol) in MeOH (0.3 mL) was then added and the solution was stirred at rt for 15 min. The resulting mixture was poured into H2O and extracted with EtOAc (×3), and the combined organic layers were washed (H2O, brine), dried (Na2SO4) and concentrated. The residue was purified by preparative HPLC (NH4OAc) to afford the title compound (0.012 g, 17%) as a colorless solid:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07348337B2 |
| Source dataset | uspto-grants-2008_03 |
| ORD ID | ord-a53c8482476d46778b9413c63d5195d0 |
| Source note | uspto-grants-2008_03 |