Hydrochloric Acid → HCID 135605572, compound

Temperature

82 °C

Acetonitril (30 ml) and 2N aqueous hydrochloric acid (23.3 ml) were added to the compound of formula (VI) obtained in Example 1-8 (1.38 g, 2.56 mmol) and stirred at 82° C. for 12 hrs with heating. After completion of the reaction, the resulting mixture was cooled to room temperature and washed with ethyl acetate to remove tritylcarbinol. The material thus obtained was neutralized to pH 6.8 by using 3N aqueous sodium hydroxide (13.6 ml) and stirred at 90° C. for 1 hr. The solution thus obtained was stirred with cooling slowly to room temperature and further stirred at room temperature for 1 hr to obtain crystal. The resulting material was cooled to 6° C. and stirred for 1 hr to obtain the title compound (0.554 g, yield: 73.1%).

1. temperaturewith heating
2. customAfter completion of the reaction
3. temperaturethe resulting mixture was cooled to room temperature
4. washwashed with ethyl acetate
5. customto remove tritylcarbinol
6. customThe material thus obtained
7. stirringstirred at 90° C. for 1 hr
8. customThe solution thus obtained
9. stirringwas stirred
10. temperaturewith cooling slowly to room temperature
11. stirringfurther stirred at room temperature for 1 hr
12. customto obtain crystal
13. temperatureThe resulting material was cooled to 6° C.
14. stirringstirred for 1 hr

ORD record

ord-30c31d11d58c44e4bf545ef91b0b1f0b

Source dataset

uspto-grants-2013_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08569491B2