反応 #73180

ord-ea79b23d79d04a57bcd85d8bc5c31064

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度with cooling, in the course of which the product
  2. 2
    その他precipitates out
  3. 3
    ろ過It is filtered off
  4. 4
    洗浄washed with 300 ml of water
  5. 5
    その他subsequently dried at 35-40° C.

実験手順

165.5 g (0.98 mol) of 2-hydroxymethyl-3-pyridinecarboxamide are heated together with 270 ml of phosphorus oxychloride to 90-100° C. for 1 hour. The reaction mixture is cooled to room temperature and subsequently added dropwise to approx. 800 ml of water at 50-60° C. After the phosphorus oxychloride has been hydrolyzed, the mixture is neutralized with sodium hydroxide solution with cooling, in the course of which the product precipitates out. It is filtered off, washed with 300 ml of water and subsequently dried at 35-40° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541450B2uspto-grants-2013_09