Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 22660706 | HCID 22660706 | — |
| Reactant | HCID 22660718 | HCID 22660718 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 22660692 | HCID 22660692 | 78% |
Reaction Steps
A mixture of 4-fluorospiro[isobenzofuran-1(3H),4′-piperidine]-3-one hydrochloride (150 mg), phenyl N-(5-phenyl-2-pyrimidinyl)carbamate (170 mg) and triethylamine (0.24 mL) in chloroform (2 mL) was stirred at 60° C. for 3 hours. The concentration of the reaction mixture left a residue, which was purified by column chromatography on silica gel (hexane/ethyl acetate/methanol=1/1/0˜8/8/1˜6/6/1) followed by recrystallization from ethyl acetate-hexane to give the subject compound(190 mg)as colorless crystals (melting point 247-249° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06803372B2 |
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| Source dataset | uspto-grants-2004_10 |
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| ORD ID | ord-9aadad0fd5304b189c22700859a4ed87 |
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| Source note | uspto-grants-2004_10 |
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