HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylmorpholine → HCID 131720343, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Reactant | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| Reactant | HCID 22879665 | HCID 22879665 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 131720343 | HCID 131720343 | 82.5% |
Reaction Steps
A mixture of N-Boc-L-leucine-L-leucine (1 g), N,O-dimethylhydroxylamine hydrochloride (423 mg), 1-hydroxybenzotriazole monohydrate (509 mg), and N-methylmorpholine (0.42 mL) was dissolved in DMF (20 mL). 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (610 mg) was added at 0° C. for 2 h, then at room temperature for 40 h. The reaction was quenched with water (80 mL) and the mixture was extracted with EtOAc (3×100 mL). The combined organic layers were washed with aqueous 10% HCl, saturated NaHCO3, and brine then dried over anhydrous MgSO4, filtered, and evaporated to afford the product (923 mg) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06660268B1 |
| Source dataset | uspto-grants-2003_12 |
| ORD ID | ord-1405d419ef1a40e09687ae1480790eb8 |
| Source note | uspto-grants-2003_12 |