HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributylphosphine → HCID 59351586, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributylphosphine | HCID 13831 | — |
| Reactant | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| Reactant | 3-Methyl-3-oxetanemethanol | HCID 137837 | — |
| Reactant | 4'-[(6-ethyl-2,4-dioxo-3,4-dihydrothieno[2,3-d]pyrimidin-1(2H)-yl)methyl]biphenyl-2-carbonitrile | HCID 59351770 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59351586 | HCID 59351586 | 56% |
Reaction Steps
A mixture of 4′-[(6-ethyl-2,4-dioxo-3,4-dihydrothieno[2,3-d]pyrimidin-1(2H)-yl)methyl]biphenyl-2-carbonitrile (1 g), 1,1′-(azodicarbonyl)dipiperidine (1.3 g), tributylphosphine (1.6 mL), (3-methyloxetan-3-yl)methanol (0.29 g) and tetrahydrofuran (30 mL) was stirred at room temperature for 3 hr. The reaction mixture was extracted with water and ethyl acetate. The ethyl acetate layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to give the title compound as a colorless amorphous solid (0.68 g, 56%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08501750B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-add952d54ed3457b83bd444330c29f55 |
| Source note | uspto-grants-2013_08 |