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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1597316Generated: October 30, 2026

Methylamine → HCID 20689431, compound

https://huagongshe.com/reaction/1597316

Reaction equation

Participants

RoleNameHCIDCharge
ReactantMethylamineHCID 6329—
ReactantPhenyl chloroformateHCID 15891—
ReactantHCID 69831129HCID 69831129—
SolventEthanolHCID 702—
ProductHCID 20689431HCID 20689431—

Reaction Conditions

Temperature110 °C

Reaction Steps

To 4-amino-5-chloro-2-methoxy-N-[1-(1-phenoxycarbonyl-4-piperidinylmethyl)-4-piperidinyl]benzamide (880 mg), which is prepared in a similar manner as in Example 1 except that phenyl chloroformate is used instead of dimethylcarbamoyl chloride, is added a 30% solution of methylamine in ethanol (20 ml), and the mixture is heated at 110° C. for 8 hours in a sealed tube. The mixture is concentrated to dryness under reduced pressure, and to the residue is added chloroform. The solution is washed with water and a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue is purified by silica gel column chromatography (eluent; chloroform:methanol=20:110:1) to give the desired compound (200 mg) as amorphous.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS06294555B1
Source datasetuspto-grants-2001_09
ORD IDord-ae3337cd38874f5494d6af2349f218a0
Source noteuspto-grants-2001_09