HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 54298263, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | tert-butyl N-[(2S)-1-hydroxy-3-phenylpropan-2-yl]carbamate | HCID 2733675 | — |
| Reactant | HCID 21266445 | HCID 21266445 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 54298263 | HCID 54298263 | — |
Reaction Steps
To a stirred mixture of 4-(3-methylphenyl)-5-(4-pyridyl)-1H-pyrid-2-one (12 mg, 0.05 mmole), (S)-2-tert-butoxycarbonylamino-3-phenylpropanol (15 mg, 0.06 mmole), triphenylphosphine (18 mg, 0.07 mmole), in methylene chloride (1 mL) at room temperature was added diethyl azodicarboxylate (12 mg, 0.07 mmol). When the reaction was complete (monitored by TLC), methanol was added (1 mL) and the reaction was concentrated and treated with 1 mL of 1:1 TFA/methanol for 30 minutes. The mixture was concentrated, neutralized with 1 drop conc NH4OH, and purified (SiO2, 10% methanol/methylene chloride) to give the title compound: MS (m/z): Calcd. C26H25N3O (M+): 395, found (M+H)+: 396.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06174901B1 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-3c3bbad8b5d74d9491e6088b53f30723 |
| Source note | uspto-grants-2001_01 |