L. Qian
2013
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Journal
Chinese Journal of Synthetic Chemistry
Abstract
O-benzylhydroxylamine hydrochloride in total yield of 90. 2% with 99. 3% purity was synthesized by amidation,etherification and hydrolysis from polyvinyl alcohol alcoholysis liquid(Ⅰ,methyl acetate content was 71% and methanol content was 28%),hydroxylamine hydrochloride( 2) and benzyl chloride( 4). The structure was confirmed by IR. Synthesis method was first reported. The optimum reaction conditions of amidation and etherification were investigated by L9( 33) and L9( 43) orthogonal experiment,respectively. The optimum amidation conditions at 40 ℃ for 3 h were as followed: 2 was 70 mmol,n( 2) ∶ n(Ⅰ) ∶ n( NaOH) was 1. 00 ∶ 2. 03 ∶ 2. 00,the yield was 95. 3%.The optimum etherification conditions at 90 ℃ for 5 h were as followed: acetylhydroxamic acid( 3)was 70 mmol,n( 3) ∶ n( 4) was 1. 00 ∶ 1. 05,DMF was 30 mL,the yield was 92. 0%.