HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tris(hydroxymethyl)aminomethane → HCID 22291576, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tris(hydroxymethyl)aminomethane | HCID 6503 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 2-Chlorobenzoyl chloride | HCID 69110 | — |
| Reactant | HCID 10158540 | HCID 10158540 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 22291576 | HCID 22291576 | 44.1% |
Reaction Steps
To a stirred solution of 8-amino-1-{4-[(dimethylamino)sulfonyl]phenyl}-4,5-dihydro-1H-benzo[g]indazole-3-carboxamide (Example 46) (1.52 g, 3.70 mmol) in pyridine (25 mL) at RT was added 2-chlorobenzoic chloride (970 mg, 5.55 mmol). After 14 h, trisamine (1 g) was added and the mixture was stirred for 2 h. The mixture was filtered through a silica gel pad with EtOAc and concentrated. Column chromatography (silica gel, EtOAc) gave the title compound as a yellow solid (900 mg, 1.63 mmol, 44%). Its structure was confirmed by 1H NMR and MS (551, M+1). C27H24ClN5O4S, Calc.: C: 58.96; H: 4.40, N: 12.73; Found, C: 58.66; H: 4.65, N: 12.58.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07186743B2 |
| Source dataset | uspto-grants-2007_03 |
| ORD ID | ord-8b47dd9c4634451c8b4e8ca93a41c3dc |
| Source note | uspto-grants-2007_03 |