HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tris(hydroxymethyl)aminomethane → HCID 10154873, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tris(hydroxymethyl)aminomethane | HCID 6503 | — |
| Reactant | 2-Chloronicotinoyl chloride | HCID 2774541 | — |
| Reactant | HCID 21092647 | HCID 21092647 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 10154873 | HCID 10154873 | 116.5% |
Reaction Steps
To a solution of title material from Example 28 (0.0791 g, 0.226 mmol) in dry pyridine (3 ml), 2-chloronicotinoyl chloride (0.0487 g, 0.2712 mmol) was added. The reaction was stirred at RT overnight. The reaction was quenched with PS-trisamine (4.61 mmol/g, 0.2021 g, 0.9318 mmol) and stirred overnight. The resins were filtrated, washed with pyridine. The combined filtrate and washes were concentrated to dryness. The resulting residue was recrystallized with hot methanol, to give 8-amino-1-[1,3-benzodioxol-5-yl]-1,4-dihydrochromeno[4,3-c]pyrazole-3-carboxamide (0.0922 g, 83.3%), which was characterized by 1H NMR, LC/MS (MH+ 489), and HPLC (96.6% purity).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07211597B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-ea203bdf38e442038c7e4c5555b4c602 |
| Source note | uspto-grants-2007_05 |