HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 69362088, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | (S)-(+)-3-Hydroxytetrahydrofuran | HCID 2733227 | — |
| Reactant | 295330-62-0 | HCID 135767195 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 69362088 | HCID 69362088 | — |
Reaction Steps
5.03 ml Diethyl azodicarboxylate are added dropwise to a solution of 8.00 g 4-[(3-chloro-4-fluoro-phenyl)amino]-6-benzyloxy-7-hydroxy-quinazoline (see WO 0055141 A1) and 2.42 ml (S)-(+)-3-hydroxy-tetrahydrofuran and 7.95 g triphenylphosphine in 160 ml tetrahydrofuran. The reaction mixture is stirred overnight at room temperature and subsequently concentrated by evaporation in the rotary evaporator. The flask residue is purified chromatographically on a silica gel column with methylene chloride/ethyl acetate (gradient from 2:1 to 1:2) as eluant.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06617329B2 |
| Source dataset | uspto-grants-2003_09 |
| ORD ID | ord-3c0024d0461146f291fc6c9790fc5e68 |
| Source note | uspto-grants-2003_09 |