Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Phenyl chloroformate | HCID 15891 | — |
| Reactant | HCID 69831129 | HCID 69831129 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 20689431 | HCID 20689431 | — |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06294555B1 |
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| Source dataset | uspto-grants-2001_09 |
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| ORD ID | ord-ae3337cd38874f5494d6af2349f218a0 |
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| Source note | uspto-grants-2001_09 |
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