Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Hydrochloride methanol | HCID 21893726 | — |
| Reactant | HCID 59171047 | HCID 59171047 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 68542650 | HCID 68542650 | 72% |
Reaction Steps
To a solution of (3S,4R)-3-cyclopropylaminomethyl-4-fluoropyrrolidine (4.74 g, 30.0 mmol) in 15 mL of methanol, 60.0 mL of a 10% hydrogen chloride-methanol solution was added dropwise over 10 minutes under stirring at room temperature. The mixture was stirred for 5 minutes. 75 mL of ethyl acetate was then added dropwise over 10 minutes and the mixture was further stirred for 10 minutes. 50 mL of ethyl acetate was further added dropwise over 10 minutes and the mixture was further stirred for 30 minutes. The resulting crystals were collected by filtration and washed with 100 mL of ethyl acetate. The washed product was dried at 50° C. under reduced pressure for 4 hours to give 4.98 g of the title compound as a faint brown crystalline powder (72% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07667049B2 |
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| Source dataset | uspto-grants-2010_02 |
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| ORD ID | ord-9ead5f6a32ce4ee6abbd98787fc41da4 |
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| Source note | uspto-grants-2010_02 |
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