Potassium Carbonate → HCID 23663550, compound

The (2S,3S)-3-[[(1S)-1-isobutoxymethyl-3-methylbutyl]carbamoyl]oxirane-2-carboxylic acid (4.83 g) prepared in Example 6 or 7 was dissolved in acetone (23 mL), and potassium carbonate (1.11 g) dissolved in water (4.5 mL) was slowly added. The solution was stirred at room temperature until the deposited inorganic salt was dissolved. While the solution was heated at 50° C. in a bath, acetone (100 mL) was dropped and a seed crystal was placed in the solution, and then the solution was stirred for 30 minutes. Acetone (94 mL) was again dropped, and the solution was stirred for 1 hour while the temperature was kept. While gradually cooled to room temperature, the solution was stirred overnight. The precipitated crystalline product was collected by filtration, washed with a mixture of 2% water-acetone (20 mL), dried in air to obtain white solid potassium (2S,3S)-3-[[(1S)-1-isobutoxymethyl-3-methylbutyl]carbamoyl]oxirane-2-carboxylate (4.28 g, 81.7%). The NMR data of the solid product were the same as those in Example 11.

1. additionwas slowly added
2. dissolutionwas dissolved
3. temperatureWhile the solution was heated at 50° C. in a bath
4. stirringthe solution was stirred for 30 minutes
5. stirringthe solution was stirred for 1 hour while the temperature
6. temperatureWhile gradually cooled to room temperature
7. stirringthe solution was stirred overnight
8. filtrationThe precipitated crystalline product was collected by filtration
9. washwashed with a mixture of 2% water-acetone (20 mL)
10. customdried in air

ORD record

ord-bbd06477b73c456babab1e3c971f75a5

Source dataset

uspto-grants-2010_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07795458B2