Yield:954238-61-0 95%

Reaction Conditions:

in tetrahydrofuran at 20; for 16 h;

Steps:

Preparation of ferf-butyl 2-bromobenzyl(methyl)carbamate (59).

Preparation of ferf-butyl 2-bromobenzyl(methyl)carbamate (59). 58 59 A solution of compound 58 (2.0 g, 10.0 mmol) and Boc₂0 (2.29 g, 10.5 mmol) in THF (40 mL) was stirred at RT for 16 hours. The mixture was then concentrated in vacuo. The crude product was purified by flash column chromatography over silica gel, which was eluted with 10% EtOAc in heptanes, and yielded compound 59 as a colorless oil (2.8 g, 95% yield). ¹H NMR (400 MHz, CDCI₃) δ 7.54 (d, 1 H), 7.30 (t, 1 H), 7.13 (m, 2 H), 4.53 (br d, 2 H), 2.87 (br s, 3 H), 1.46 (br d, 9 H).

References:

WO2013/132376,2013,A1 Location in patent:Page/Page column 167