反应 #1597026

ord-93f89fb81e304d95a9938164b421c2f5

反应方程式

COC(=O)c1cccc(-c2ncc(N=CN(C)C)cn2)c1
methyl 3-[5-(dimethylaminomethylenamino)pyrimidin-2-yl]benzoate
O=S(=O)(O)O
sulfuric acid
O=C(O)c1cccc(-c2ncc(O)cn2)c1
3-(5-hydroxypyrimidin-2-yl)benzoic acid

溶剂

反应条件

温度
130°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度For work-up, the reaction batch is cooled
  2. 2
    其他the precipitate formed
  3. 3
    过滤is filtered off
  4. 4
    洗涤washed with water
  5. 5
    其他dried at 50° C. in a vacuum
  6. 6
    其他drying cabinet

实验过程

103.5 g of methyl 3-[5-(dimethylaminomethylenamino)pyrimidin-2-yl]benzoate (364.04 mmol) are suspended in 1300 ml of water in a 2 l single-necked flask, and 160 ml of conc. sulfuric acid (95-97%) (2.88 mol) are subsequently added, and the reaction batch is warmed at 130° C. (oil-bath temperature) for 4 h. For work-up, the reaction batch is cooled, and the precipitate formed is filtered off, washed with water and dried at 50° C. in a vacuum drying cabinet.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08211886B2uspto-grants-2012_07