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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 516234Generated: October 30, 2026

Water → HCID 58494744, compound

https://huagongshe.com/reaction/516234

Reaction equation

Participants

RoleNameHCIDCharge
ReactantWaterHCID 962—
ReactantMethyl iodideHCID 6328—
ReactantPotassium CarbonateHCID 11430—
ReactantHCID 66982532HCID 66982532—
SolventDimethylformamideHCID 6228—
ProductHCID 58494744HCID 5849474443.9%

Reaction Steps

To a solution of 120 mg of t-butyl 2-methyl-3,4,6,7,9,10-hexahydro[1,4]oxazino[2,3-h][3]benzazepine-8(2H)-carboxylate in 4 ml of DMF were added 0.026 ml of methyl iodide and 104 mg of potassium carbonate at room temperature, followed by stirring for 13 hours. To the reaction mixture were added 0.012 ml of methyl iodide and 26 mg of potassium carbonate, followed by further stirring for 3 hours. To the reaction mixture was added water, followed by extraction with EtOAc twice. The combined organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and then filtered, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography (elution solvent: HEX-EtOAc) to obtain 55 mg of t-butyl 2,4-dimethyl-3,4,6,7,9,10-hexahydro[1,4]oxazino[2,3-h][3]benzazepine-8(2H)-carboxylate as a brown solid.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09108977B2
Source datasetuspto-grants-2015_08
ORD IDord-dbb1ec7dfdfa46159a76c2530f773cca
Source noteuspto-grants-2015_08