HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Hydroxybenzotriazole → HCID 69878533, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Reactant | 3-Amino-2-methylbenzoic acid | HCID 2733699 | — |
| Reactant | HCID 69879159 | HCID 69879159 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 69878533 | HCID 69878533 | 64.2% |
Reaction Steps
EDC.HCl (42 mg) was added to a solution of the compound obtained in Step 2 of Example 1 (94 mg), 3-amino-2-methylbenzoic acid (30 mg), and HOBt (27 mg) in DMF while cooling with ice, and the mixture was stirred overnight. EtOAc was added and the mixture was washed with 5% Na2CO3 (×2) and 5% NaCl, dried over MgSO4, filtered and concentrated. The residue was purified by silica gel column chromatography (CH2Cl2—MeOH) and reprecipitated from a mixture of CH2Cl2 and n-hexane to obtain the title compound (77 mg, 64%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06673772B2 |
| Source dataset | uspto-grants-2004_01 |
| ORD ID | ord-0c08a5a880644af880251066c53f0961 |
| Source note | uspto-grants-2004_01 |