HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 71290288, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| Reactant | 3,3,3-Trifluoro-1-propanol | HCID 137512 | — |
| Reactant | HCID 178429273 | HCID 178429273 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 71290288 | HCID 71290288 | — |
Reaction Steps
Under argon, 80 mg (0.19 mmol) of the compound from example 31 was largely dissolved in 2 ml THF, 32.5 mg (0.29 mmol) of 3,3,3-trifluoropropan-1-ol, 75 mg (0.29 mmol) of triphenyl phosphine and 56 μl (0.29 mmol) of diisopropyl azodicarboxylate were added and it was stirred for 3 d at RT. A further 11 mg (0.01 mmol) of 3,3,3-trifluoropropan-1-ol, 25 mg (0.01 mmol) of triphenyl phosphine and 19 μl (0.01 mmol) of diisopropyl azodicarboxylate were added and it was stirred for 1 d at RT. The reaction mixture was concentrated by evaporation and the residue was purified by preparative HPLC (Reprosil C18, gradient of acetonitrile/0.01% aq. formic acid). Yield: 48 mg (49% of theor.)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08859569B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-0be01bc5078e4583a9d66b6fdb144cba |
| Source note | uspto-grants-2014_10 |