Hydrochloric Acid → HCID 70673857, compound

Temperature

40 °C

To a solution of 4-ethoxy-N-(2-fluoroethyl)-N,N-dimethyl-4-oxobutan-1-aminium chloride (4) from the preceding step (3.61 g, ≦514.2 mmol) in dioxane (10 ml) was added conc. HCl (5 ml) and the reaction mixture was stirred at 40° C. for 24 h. The mixture was evaporated, to the residue (3.02 g) was added conc.HCl (15 ml) and stirred at 70° C. for 2 h, then the mixture was evaporated again. The residue was triturated with acetonitrile in an ultrasound bath, then the mixture was decanted and the crystalline solid was washed with acetone. After drying in vacuo over P2O5 2.125 g of the 3-carboxy-N-(2-fluoroethyl)-N,N-dimethylpropan-1-aminium chloride (6) was obtained.

1. customThe mixture was evaporated, to the residue (3.02 g)
2. additionwas added conc
3. stirringHCl (15 ml) and stirred at 70° C. for 2 h
4. customthe mixture was evaporated again
5. customThe residue was triturated with acetonitrile in an ultrasound bath
6. customthe mixture was decanted
7. washthe crystalline solid was washed with acetone
8. dry with materialAfter drying in vacuo over P2O5 2.125 g of the 3-carboxy-N-(2-fluoroethyl)-N,N-dimethylpropan-1-aminium chloride (6)
9. customwas obtained

ORD record

ord-ff7f12bbf55b4eae9680ca4c98da7c5d

Source dataset

uspto-grants-2015_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08940793B2