HuagongsheHuagongshe Chemistry Print Report · For research reference only
Indazole-3-carboxylic acid → 1H-Indazole-3-carboxylic acid (4-benzyloxy-phenyl)-amide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Indazole-3-carboxylic acid | HCID 78250 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 4-Benzyloxyaniline hydrochloride | HCID 2723831 | — |
| Reactant | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 1H-Indazole-3-carboxylic acid (4-benzyloxy-phenyl)-amide | HCID 9314292 | — |
Reaction Steps
DIEA (9.3 mL, 53.4 mmol) was added to a solution of 4-benzyloxyaniline hydrochloride (4.0 g, 17.0 mmol), indazole-3-carboxylic acid (2.89 g, 17.8 mmol) and HBTU (7.1 g, 18.7 mmol) in DMF (60 mL), and the resulting solution was stirred at ambient temperature for 24 hours. The solution was heated to 70° C. for 4 hours, and then poured into a mixture of saturated aqueous sodium bicarbonate on ice. The product, an off white solid, 6.0 g, was collected by filtration, washed with water and used without further purification in the subsequent reaction. MS m/z 344 (MH+). 1H NMR(DMSO-d6) δ 5.11 (s, 2H), 7.02 (d, 2H), 7.26-7.48 (m, 7H), 7.67 (d, 1H), 7.75 (d, 2H), 7.81 (d, 1H), 8.24 (d, 1H) and 10.24 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07718692B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-9f635631f26e4031b0e909c34f052475 |
| Source note | uspto-grants-2010_05 |