Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyrrolidine | HCID 31268 | — |
| Reactant | 4-chloropyridine-2,6-dicarboxylic acid | HCID 304010 | — |
| Product | HCID 86714237 | HCID 86714237 | — |
Reaction Steps
4-chloropyridine-2,6-dicarboxylic acid (0.238 mol, 48.0 g) is slowly added under stirring to a solution of pyrrolidine (0.952 mol, 67.8 g) at room temperature. Take care to avoid a too-fast addition leading to local temperature increase. Observe precipitation of a solid. The reaction mixture is heated at 120° C. for 2 hr. By gradually heating, the reaction mixture becomes solid. After cooling at 60° C., H20 (80 ml) is added and the mixture is stirred for 30 min until the solid is completely dissolved. The solution is then acidified with HCl (2M) until pH=1. The formed precipitate is filtered, washed twice H2O and dried overnight at 70° C. (93%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09163155B2 |
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| Source dataset | uspto-grants-2015_10 |
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| ORD ID | ord-5fbc7338f31c444cb0443bee179158cb |
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| Source note | uspto-grants-2015_10 |
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