HuagongsheHuagongshe Chemistry Print Report · For research reference only
Imidazole → tert-butyl 2-(2-hydroxy-N-methylbenzamido)ethylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | Dicyclohexylcarbodiimide | HCID 10868 | — |
| Reactant | Salicyloyl chloride | HCID 74041 | — |
| Reactant | N-(tert-Butoxycarbonyl)-N'-methylethylenediamine | HCID 3435744 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | tert-butyl 2-(2-hydroxy-N-methylbenzamido)ethylcarbamate | HCID 59193319 | 34% |
Reaction Steps
To a mixture of tert-butyl 2-(methylamino)ethylcarbamate (0.348 g, 2 mmol), 2-hydroxybenzoyl chloride (0.276 g, 2 mmol) and imidazole (0.136 g, 2 mmol) in ethyl acetate (8 mL) at 0° C. was slowly added a solution of DCC (0.412 g, 2 mmol) in ethyl acetate (2 mL). The mixture was stirred (RT, 16 h), filtered and concentrated under reduced pressure. The crude material was purified by chromatography on silica gel, eluting with ethyl acetate/petroleum ether (20-50%) to afford tert-butyl 2-(2-hydroxy-N-methylbenzamido)ethylcarbamate (0.2 g, 34%) as a colorless oil. 1HNMR (CDCl3): δ7.5 (m, 2H, CH), 7.0 (d, 1H, CH), 6.8 (d, 1H, CH), 3.7 (m, 2H, CH2), 3.48 (m, 2H, CH2), 3.2 (m, 3H, CH3), 1.5 (s, 9H, CH3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09272984B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-79cf56cb1fd5405e981d9d3d146f20e8 |
| Source note | uspto-grants-2016_03 |