Hydrochloric Acid → HCID 58018315, compound

Temperature

10 °C

Water (21 mL), acetone (9.80 mL) and a 6M sodium hydroxide aqueous solution (5.20 mL) were added to 7.50 g of 4-iodo-L-phenylalanine and the resulting mixture was stirred at 10° C. to thus give a uniform solution. To this solution, there were alternatively added 4.05 mL of 2,6-dichlorobenzoyl chloride and 4.50 mL of a 6M sodium hydroxide aqueous solution while taking care to maintain the pH value of not less than 13 and the temperature of not higher than 15° C. After confirming the completion of the reaction, 6.50 mL of a 6M hydrochloric acid aqueous solution was added to the reaction system to thus precipitate the desired product. The solid thus separated was isolated through filtration under reduced pressure, washed with 15 mL of water and dried at 70° C. for 4 hours under reduced pressure to thus give 12.42 g of the intended product.

1. customto thus give a uniform solution
2. temperatureto maintain the pH value of not less than 13
3. customhigher than 15° C
4. additionwas added to the reaction system
5. customto thus precipitate the desired product
6. customThe solid thus separated
7. customwas isolated through filtration under reduced pressure
8. washwashed with 15 mL of water
9. dry with materialdried at 70° C. for 4 hours under reduced pressure to thus give 12.42 g of the intended product

ORD record

ord-e3139f1524d74b8a98a8250753f802cd

Source dataset

uspto-grants-2013_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08546610B2