Yield:90537-30-7 91%

Reaction Conditions:

with formic acid;sodium formate at 95 - 120; for 7 h;

Steps:

4.1.1.4.4

Synthesis of 3-chloro-4,5-dimethoxy-benzonitrile (4.4) (for Example 6, 7, 9)4.410 g 3-Chloro-4,5-dimethoxybenzaldehyde, 7.3 g sodium formate in 50 mL formic acid was stirred at 95°C. Hydroxylamine hydrochloride was added in portions and the mixture stirred for 4 h at 95°C and 3 h at 120°C. The formic acid was almost distilled off and the residue was suspended in water. This was added to 700 mL almost saturated sodium chloride solution and the precipitate isolated, washed with water and dried.Yield: 9 g (91 % of theory)Analysis: HPLC-MS (method E): R_t: 1 .23 min.

References:

WO2011/92128,2011,A1 Location in patent:Page/Page column 35