Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | HCID 53707904 | HCID 53707904 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 54378998 | HCID 54378998 | 60.2% |
Reaction Steps
550 mg of 6-benzyl-2,6-diazaspiro[3,4]octane-8-one-O-methyloxime was added to 10 ml of ethanol and thereto 0.4 ml of acetic acid and 176 mg of paraformaldehyde were added and the resulting mixture was stirred for 30 minutes at room temperature and thereto 370 mg of sodium cyanoborohydride was added. The resulting mixture was stirred for 16 hours at room temperature, neutralized with aqueous solution of potassium carbonate and distilled under the reduced pressure and the obtained residue was added into 50 ml of dichloromethane, washed with 50 ml of water, dried with magnesium sulfate, filtered and concentrated under the reduced pressure. The residue was purified by silicagel column chromatography(methanol:normal hexane:dichloromethane=1:10:8) to give 350 mg of the titled compound(yield: 60.1%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06313299B1 |
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| Source dataset | uspto-grants-2001_11 |
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| ORD ID | ord-b26fe753a6bc4ef3979db7fab4d5935b |
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| Source note | uspto-grants-2001_11 |
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