反应详情

温度

75 °C

Methyl N-(3-chloro-4-fluorophenyl)-4-[(triisopropylsilyl)oxy]methyl-1,2,5-oxadiazole-3-carbimidothioate (3.0 g, 6.5 mmol) was dissolved in EtOH followed by addition of 4 mL hydroxylamine (99.9% in water solution). The reaction was stirred at 75° C. for 6 hrs and monitored by HPLC. The reaction was concentrated in vacuo to a yellow oil which was dissolved in chloroform and chromatographed on 120 g of silica gel eluting with (1:4), EtOAc/hexane. The product was concentrated to give the desired product as a white solid (2.57 g, 89%); MF=C19H28ClFN4O3Si; LCMS calculated for C19H29ClFN4O3Si(M+H)+: m/z=443.168.

1. concentrationThe reaction was concentrated in vacuo to a yellow oil which
2. dissolutionwas dissolved in chloroform
3. customchromatographed on 120 g of silica gel eluting with (1:4), EtOAc/hexane
4. concentrationThe product was concentrated