5-AMINO-4-CHLORO-2-METHYLPHENYL ETHYL CARBONATE synthesis

Yield:930298-25-2 85%

Reaction Conditions:

with water;iron;acetic acid at 85; for 1.5 h;

Steps:

27.3

Iron powder (7.8 g) was added to a suspension of carbonic acid 4-chloro-2-methyl-5- nitro-phenyl ester ethyl ester (7.23 g) in Acetic acid (75 ml) and water (37 ml). Reaction mixture was heated to 85 ⁰C for 90 mins. The hot suspension was filtered through a pad of celite and filtrate allowed to cool. Water was added and the mix was EPO extracted with dichloromethane. The organic phase was washed with 2N NaOH solution (aq) then sat NaCI (aq) solution and dried over MgSO₄. Mixture was filtered and filtrate solvents removed in vacuo to afford product as a brown oil, (5.448 g, 85%).

References:

WO2007/34185,2007,A1 Location in patent:Page/Page column 44-45