HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Hydroxybenzotriazole → HCID 86720745, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Reactant | HCID 19786348 | HCID 19786348 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 86720745 | HCID 86720745 | 100.6% |
Reaction Steps
To a N,N-dimethylformamide (25 mL) solution of 5-tert-butyl-1,3-thiazole-2-carboxylic acid (2.5 g), N,O-dimethylhydroxylamine hydrochloride (2.0 g), WSC.HCl (3.9 g), HOBt.H2O (3.1 g) and triethylamine (7.1 g) were added, and the resultant was stirred at room temperature for 1 day. Water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was dried over magnesium sulfate, and the desiccant was filtered off. Then, the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography (NH-type silica gel; hexane/ethyl acetate-gradient elution=100/0→50/50) to obtain the title compound (3.1 g) as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09045466B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-5f0977a9ae7e4b6f96608a7d580d4d31 |
| Source note | uspto-grants-2015_06 |