Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | 4-Chlorobenzoyl chloride | HCID 8501 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 28958339 | HCID 28958339 | — |
| Solvent | Chlorobenzene | HCID 7964 | — |
| Product | HCID 59294609 | HCID 59294609 | 49.5% |
Reaction Steps
To the aqueous solution of (R)-1-(p-chlorobenzoyl)-3-amino piperidine obtained in Example 14 (amount: 3 g), p-chlorobenzoyl chloride (0.15 g) was added. The pH of the mixture was kept from pH 8.0 to 9.0 using sodium hydroxide. The mixture was stirred at 15° C. for 3 hours, and chlorobenzene (3 ml) and sodium chloride (0.5 g) were added. The mixture was stirred at 90° C. for 10 minutes. The water layer was removed, and the solvent was evaporated under reduced pressure to obtain the title compound as yellow crystal (0.16 g, yield: 36%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08338142B2 |
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| Source dataset | uspto-grants-2012_12 |
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| ORD ID | ord-846ec0c125b344a7a925a88b67fb88ea |
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| Source note | uspto-grants-2012_12 |
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