Hydrochloric Acid → HCID 86688558, compound

20.0 mL 4N HCl in dioxane are added to 17.2 g (53.4 mmol) 2-methyl-propane-2-sulfonic acid [1-(4-bromo-3-fluoro-phenyl)-ethyl]-amide (X.1) in 150 mL MeOH. Stirring is continued for 1 h. After that time, the mixture is concentrated and the residue is triturated from diethylether (150 mL). The precipitate is filtered off, washed with diethylether and suspended in 250 mL DCM. 8.64 mL (107 mmol) pyridine and 5.29 mL (56.1 mmol) acetic anhydride are added and the mixture is stirred for 12 h at rt. After that time, the mixture is transferred to a separation funnel, washed with 1N HCl (200 mL) and sat. aq. NaHCO3-solution (200 mL) and dried over sodium sulphate. The solvent is removed by evaporation to yield the desired product.

1. concentrationAfter that time, the mixture is concentrated
2. customthe residue is triturated from diethylether (150 mL)
3. filtrationThe precipitate is filtered off
4. washwashed with diethylether
5. stirringthe mixture is stirred for 12 h at rt
6. customAfter that time, the mixture is transferred to a separation funnel
7. washwashed with 1N HCl (200 mL) and sat. aq. NaHCO3-solution (200 mL)
8. dry with materialdried over sodium sulphate
9. customThe solvent is removed by evaporation

ORD record

ord-3204712d12ea4d178861ec163e44d225

Source dataset

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08765959B2