HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 22667046, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | HCID 3030629 | HCID 3030629 | — |
| Reactant | HCID 135674211 | HCID 135674211 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22667046 | HCID 22667046 | 42% |
Reaction Steps
N-{2-Chloro-4-[(7-hydroxy-6-methoxy-4-quinazolinyl)oxy]phenyl}-N′-ethylurea (2.7 g) was dissolved in N,N-dimethylformamide (30 ml), and triphenylphosphine(3.6 g), piperidinopropanol (1.2 g), and diethyl azodicarboxylate (2.4 g) were added to the solution. The mixture was stirred at room temperature for 2 hr. Triphenylphosphine(3.6 g), piperidinopropanol (0.8 g), and diethyl azodicarboxylate (1.9 g) were then again added to the reaction solution. The mixture was stirred at room temperature for additional 10 hr. The solvent was removed by distillation under the reduced pressure, and the residue was purified by chromatography on silica gel by development with chloroform/methanol (20/1) to give 1.5 g (yield 42%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07169789B2 |
| Source dataset | uspto-grants-2007_01 |
| ORD ID | ord-9f1a098909ce4b2489b74ffb943935ea |
| Source note | uspto-grants-2007_01 |