反应详情

A solution of m-bromobenzonitrile (1.82 g; 10 mmol) in MeOH (20 mL) at 0° C. was sparged with HCl gas for 30 min, the reaction flask was stoppered and aged in a refrigerator (ca. 5° C.) for 3 h. The mixture was sparged with N2 to remove excess HCl, concentrated in vacuo (2×PhMe chase) and dried under high vacuum ca. 45 min, affording the title compound as a colorless solid which was used directly for Step 2 below. LC/MS (method A) tR 0.81 min, m/z 214, 216 (M+H, Br isotopes).

1. customThe mixture was sparged with N2
2. customto remove excess HCl
3. concentrationconcentrated in vacuo (2×PhMe chase)
4. customdried under high vacuum ca. 45 min