Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Malonic Acid | HCID 867 | — |
| Reactant | Sibutramine | HCID 5210 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86614367 | HCID 86614367 | 92.8% |
Reaction Steps
15 g of sibutramine was dissolved in 60 ml of ethyl acetate. Malonic acid (5.72 g) dissolved in 20 ml ethyl acetate was slowly added in droplets to the sibutramine solution at room temperature and agitated for 2 hrs. The resulting solution was cooled to 0° C., agitated for about 2 hrs, and filtered to collect a deposited crystal. The crystal was washed with 50 ml of isopropyl ether and vacuum-dried at 50° C., thus obtaining 19 g (yield: 92.6%) of a white target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07393977B2 |
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| Source dataset | uspto-grants-2008_07 |
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| ORD ID | ord-cefbae68aeb34da7b313290c6ac65641 |
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| Source note | uspto-grants-2008_07 |
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