HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 178525420, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 2,2-Bis(6-benzyloxyhexyl)acetic acid | HCID 18920839 | — |
| Reactant | N-ethoxycarbonyliminocarbamate | HCID 86599450 | — |
| Reactant | HCID 178520594 | HCID 178520594 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178525420 | HCID 178525420 | 97.1% |
Reaction Steps
First, 3 g of 2,3-difluoro-1-[trans-4-(13-hydroxytridecyl)cyclohexyl]benzene, 3 g of 2,2-bis(6-benzyloxyhexyl)acetic acid, 2.2 g of triphenylphosphine, and 30 ml of tetrahydrofuran were placed in a 100 ml flask. Then, 1.5 g of ethyl azodicarboxylate was added dropwise to the reaction mixture under ice water cooling. The reaction mixture was allowed to warm to room temperature and stirred for 2 hours. The reaction mixture was concentrated, and the residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=9/1) to obtain 5.4 g of 13-[trans-4-(2,3-difluorophenyl)cyclohexyl]tridecyl 2,2-bis(6-benzyloxyhexyl)acetate (Y: 97%). The compound thus obtained had a purity of 93.7% by HPLC.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05750213 |
| Source dataset | uspto-grants-1998_05 |
| ORD ID | ord-685ff8f05552457184677eb8e5651e4b |
| Source note | uspto-grants-1998_05 |