HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 54427559, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | tert-butyl N-(3-hydroxypropyl)carbamate | HCID 3838134 | — |
| Reactant | HCID 53769834 | HCID 53769834 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 54427559 | HCID 54427559 | 67.7% |
Reaction Steps
A solution of 3-[(tert-butoxycarbonyl)amino]-1-propanol (0.14 g, 0.8 mmol) and diethyl azodicarboxylate (0.13 mL, 0.8 mmole) in anhydrous DMF (2 mL) was added dropwise to a solution of methyl (±)-8-hydroxy-3-oxo-2,3,4,5-tetrahydro-1H-2-benzazepine-4-acetate (0.10 g, 0.4 mmole) and triphenylphosphine (0.21 g, 0.8 mmol) in anhydrous DMF (1.4 mL) and dry THF (2 mL) at RT under argon. The resulting solution was stirred for 18 hr, then was concentrated under vacuum. Silica gel chromatography (1%-3% MeOH/CH2Cl2) gave the title compound (0.11 g): MS (ES) m/e 407.3 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06825188B2 |
| Source dataset | uspto-grants-2004_11 |
| ORD ID | ord-9191ed60335d42b38b445e5a3204eeac |
| Source note | uspto-grants-2004_11 |