Hydrochloric Acid → HCID 118054698, compound

To a solution of (S)—N—((S)-2-amino-1-(3-bromo-5-fluorophenyl)ethyl)-2-methylpropane-2-sulfinamide (100 mg, 0.297 mmol) in DCM (988 μl) was added TEA (124 μl, 0.890 mmol) and methyl chloroformate (24.12 μl, 0.311 mmol). The reaction mixture was stirred at room temperature for 1 h. The reaction mixture was extracted by EtOAc and the organics were washed with water and brine, dried over sodium sulfate, filtered off, and concentrated in vacuo. The residue was dissolved in Et2O (1 mL), then HCl (4M in dioxane) (148 μl, 0.593 mmol) was added. The reaction mixture was stirred at room temperature for 30 min. After the solvent was decant out, the residue solid was used in next step without further purification. LCMS (m/z): 291.2/293 (MH+), 0.49 min.

1. extractionThe reaction mixture was extracted by EtOAc
2. washthe organics were washed with water and brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltered off
5. concentrationconcentrated in vacuo
6. dissolutionThe residue was dissolved in Et2O (1 mL)
7. stirringThe reaction mixture was stirred at room temperature for 30 min
8. customAfter the solvent was decant out
9. customthe residue solid was used in next step without further purification
10. custom291.2/293 (MH+), 0.49 min.

ORD record

ord-4a35a45b707744d4a23a8ac12ce31763

Source dataset

uspto-grants-2016_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09242996B2