TERT-BUTYL 4-IODO-2-METHYLPHENYLCARBAMATE synthesis

Yield:666746-27-6 99%

Reaction Conditions:

in toluene at 80; for 16 h;

Steps:

A1.1; A11.1; A12.1 Step 1: (4-iodo-2 -methyl -phenyl)-carbamic acid tert-butyl ester

To a mixture of 4-iodo-2-methyl-phenylamine (1.29 g, 5.5 mmol) in toluene (40 mL) was added B0C2O (1.81 g, 8.3 mmol). The resulting mixture was then heated at 80°C for 16 h. The solvent was removed in vacuum and the residue was purified by silica gel column chromatography (PE to PE/EA = 20/1) to give (4-iodo-2-methyl-phenyl)-carbamic acid tert- butyl ester (1.8 g, 99% yield) as white solid. NMR (300 MHz, CDCh): d = 7.64 (d, J= 9.7 Hz, 1H), 7.55 - 7.41 (m, 2H), 6.24 (brs, 1H), 2.21 (s, 3H), 1.53 (s, 9H). MS: m/z 334.0 (M⁺H⁺ ).

References:

WO2021/50547,2021,A1 Location in patent:Paragraph 0103-0105; 0142-0144; 0151-0153