Ethyl Acetate → HCID 68542650, compound

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).

1. stirringThe mixture was stirred for 5 minutes
2. stirringthe mixture was further stirred for 10 minutes
3. stirringthe mixture was further stirred for 30 minutes
4. filtrationThe resulting crystals were collected by filtration
5. washwashed with 100 mL of ethyl acetate
6. customThe washed product was dried at 50° C. under reduced pressure for 4 hours

ORD record

ord-9ead5f6a32ce4ee6abbd98787fc41da4

Source dataset

uspto-grants-2010_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07667049B2