تفاعل #79540

ord-ce3bacdc51c043e1bb44ad49b17a2372

المذيبات

ظروف التفاعل

درجة الحرارة
40°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحthe solution was filtered
  2. 2
    غسيلthe catalyst washed with 108 g of methanol which
  3. 3
    workup.ADDITIONwas added to the filtrate

الإجراء التجريبي

A 1-L Parr reactor was charged with 12.43 g (0.051 mol) of 4-[1-hydroxy-1-(2,3-dimethoxyphenyl)methyl]pyridine (10), 5.74 g of a 5% Rhodium on Carbon catalyst, and 237 g of methanol. The solution was warmed to 40° C. and treated with 100 psi of hydrogen for 5.5 h. When the reaction was complete, the solution was filtered and the catalyst washed with 108 g of methanol which was added to the filtrate. The weight of the filtered solution was 310.45 g. The methanol solution was assayed for the title compound using high pressure liquid chromatography. The methanol solution was found to contain 3.7% title compound by weight. This corresponds to 11.5 g (90% yield) of title compound.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06713627B2uspto-grants-2004_03