R-3-Nitrophenylglycine synthesis

Yield: 96.8%

Reaction Conditions:

with sulfuric acid;nitric acid at 50; for 6.5 h;Cooling with ice;

Steps:

1
To an ice bath cooled solution of nitric acid - sulfuric acid (volume ratio 1: 4) mixed acid 45mL, and added slowly portionwise D- phenylglycine (R-Phg-H) lOOmmol, after stirring for 0.5 hours, 50 ° C water bath with stirring The reaction 6.5 hours. After completion of the reaction, the reaction mixture was added a small amount of ice-water mixture, at ice bath with concentrated aqueous ammonia to adjust the pH to 5-6, a heavy precipitate precipitated, suction filtered, the filter cake washed with ice-water (lXlOmL), ethanol (2X10 mL), oil ether (lXlOmL), ethanol (lXlOmL), dried, affording intermediate DMl (pale yellow solid) 18. 894g, a yield of 96.8%.

References:

Southwest University;Yang, DACHENG;CHEN, XIN;FAN, LI;Li, HUACHONG;Su, XIAOYAN;DENG, YUBI;Xiao, LIJUAN CN103570586, 2016, B Location in patent:Paragraph 0051-0052