HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-(Trifluoromethyl)phenol → HCID 23502796, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-(Trifluoromethyl)phenol | HCID 7376 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | HCID 10299574 | HCID 10299574 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 23502796 | HCID 23502796 | 60% |
Reaction Steps
A solution of 80 mg (0.17 mmol) N-(3,5-bis-trifluoromethyl-benzyl)-6-hydroxymethyl-N-methyl-4-o-tolyl-nicotinamide (Example 7), 0.027 ml (0.22 mmol) 3-hydroxybenzotrifluoride, 47 mg (0.17 mmol) triphenylphosphine and 32 mg (0.17 mmol) diethyl azodicarboxylate in 2 ml tetrahydrofuran was stirred at room temperature over night. The reaction mixture was diluted with ethyl acetate and washed with 1N aqueous sodium hydroxide solution. The aqueous layer was extracted with three portions of ethyl acetate. The combined organic extracts were dried with sodium sulfate and concentrated. Column chromatography afforded 62 mg (60%) of the title compound as a light yellow amorphous mass.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06770637B2 |
| Source dataset | uspto-grants-2004_08 |
| ORD ID | ord-ab79a4dde9e243bd9c02ce13e5667d18 |
| Source note | uspto-grants-2004_08 |