HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-(Trifluoromethoxy)benzoic acid → HCID 131727927, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-(Trifluoromethoxy)benzoic acid | HCID 67613 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HOAt | HCID 181649 | — |
| Reactant | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| Reactant | HCID 131727924 | HCID 131727924 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 131727927 | HCID 131727927 | — |
Reaction Steps
To a solution of the material prepared in Step B of Example 24 (0.020 g, 0.054 mmol) in DMF (2 mL) was added 4-(trifluoromethoxy)benzoic acid (0.0090 g, 0.059 mmol), HOAT (0.0080 g, 0.059 mmol), N,N-diisopropylethylamine (0.047 mL, 0.27 mmol) and HATU (0.022 g, 0.059 mmol). After 24 h at ambient temperature the reaction was diluted with 100 mL of ethyl acetate and washed with 100 mL of 0.5 M aqueous sodium bicarbonate. The organic layer was washed with brine, dried (magnesium sulfate) and concentrated in vacuo. Purification by reverse phase HPLC (30%-60% acetonitrile in H20 gradient) afforded the title compound as a white solid. LC/MS 506.3 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07671073B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-41b1da3bee544468b93c0617d28ff8ec |
| Source note | uspto-grants-2010_03 |