HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanamine, N-methoxy-, hydrochloride (1:1) → HCID 88414359, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| Reactant | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| Reactant | HCID 70663716 | HCID 70663716 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 88414359 | HCID 88414359 | 91.9% |
Reaction Steps
A solution of the compound of example 8, step 11 (1.002 g, 1.75 mmol), N,O-dimethylhydroxylamine hydrochloride (0.213 g, 2.19 mmol), EDIA (0.76 ml, 4.38 mmol) and TBTU (0.702 g, 2.19 mmol) in 15 ml of anhydrous DCM was stirred at room temperature for 4 h. DCM (15 ml) was then added and the solution was washed with 0.5 N hydrochloric acid (30 ml), a saturated solution of sodium hydrogencarbonate (15 ml) and brine (15 ml), dried over magnesium sulfate, filtered and evaporated to dryness under reduced pressure. The residue was purified by chromatography on silica gel (cyclohexane/EA, 50:50, then 40:60, then 35:65) to give 0.99 g of the title compound as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08415336B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-2a14668604c14fddbf01adc727491152 |
| Source note | uspto-grants-2013_04 |