Yield:60541-86-8 83%

Reaction Conditions:

with dichlorosulfoxide at 0 - 85; for 16 h;

Steps:

F14 Preparation of Example F14: 2-(2,5-dichloro-3-(chlorosulfonyl)phenyl)propan-2-yl acetate

A solution of 3-amino-2,5-dichlorobenzoic acid (14.0 g, 68.0 mmol) in EtOH (120 mL) was cooled to 0 C and thionyl chloride (20.0 mL, 169 mmol) was added dropwise. The reaction mixture was further heated at 85 C for 16 h. The reaction mixture was cooled to rt and concentrated under reduced pressure. The crude was triturated with n-pentane to afford ethyl 3-amino-2,5- dichlorobenzoate (14.0 g, 83% yield) as brown solid.¹H NMR (500 MHz, DMSO-d6): δ 6.96 (d, J = 2.4 Hz, 1H), 6.85 (d, J = 2.4 Hz, 1H), 5.96 (brs, 2H), 4.29 (q, J = 7.2 Hz, 2H), 1.29 (t, J = 6.8 Hz, 3H).

References:

WO2022/109001,2022,A1 Location in patent:Paragraph 0308