HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylmorpholine → HCID 86632571, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| 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 | N-((1,1-dimethylethoxy)carbonyl)-2-methyl-alanine | HCID 2733845 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86632571 | HCID 86632571 | — |
Reaction Steps
To a solution of 2-tert-butoxycarbonylamino-2-methyl-propionic acid (8.0 g, 39 mmol) and N,O-dimethylhydroxylamine hydrochloride (4.6 g, 47 mmol) in methylene chloride (80 mL) is added N-methylmorpholine (5.2 mL, 47 mmol), HOBT (6.4 g, 47 mmol) and EDCl (9.1 g, 47 mmol). The mixture is stirred at RT for 18 h then is washed sequentially with 10% citric acid (2×), sat. NaHCO3 (2×) and brine. The organic solution is dried over magnesium sulfate and the solvent removed under reduced pressure. The resulting oil is purified by flash chromatography to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08084448B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-6bdcf4b66bee4cd88e5f822111ad4440 |
| Source note | uspto-grants-2011_12 |