Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | 4-Methylbenzoyl Chloride | HCID 13405 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 3-Piperidinecarboxamide | HCID 92980 | — |
| Product | HCID 59294624 | HCID 59294624 | 34.5% |
Reaction Steps
Concentrated sulfuric acid is added to the reaction mixture obtained in Example 4 (amount: 30 g, net weight of (R)-nipecotamide: 3 g) to adjust the pH to 9. To the mixture, p-Methylbenzoyl chloride (8.0 g, 2.2 equivalents) was slowly added dropwise, and the pH of the reaction mixture was kept from 7 to 9 by a 30% aqueous sodium hydroxide solution. After completion of the dropwise addition, the solution was stirred at 15° C. for 3 hours and the precipitated crystal was filtered off. The crystal was dried under reduced pressure to obtain the title compound as white crystal (4.4 g, yield: 760).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08338142B2 |
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| Source dataset | uspto-grants-2012_12 |
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| ORD ID | ord-3dfe8877735943a38dd7655a65a3fa2f |
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| Source note | uspto-grants-2012_12 |
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