反应 #417978

ord-61a0a40cb8dc40a0a3e9bca79d2008e7

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the mixture is heated at the boil for 4 hours
  2. 2
    过滤filtered off with suction
  3. 3
    洗涤The residue is washed with water
  4. 4
    其他dried in vacuo
  5. 5
    其他=2.19 min (method A)

实验过程

160 ml (2.88 mol) of concentrated sulfuric acid are added to a suspension of 103.5 g (364 mmol) of methyl 3-[5-(dimethylaminomethyleneamino)pyrimidin-2-yl]benzoate in 1.3 l of water, and the mixture is heated at the boil for 4 hours. The reaction mixture is cooled to room temperature, diluted with water and filtered off with suction. The residue is washed with water and dried in vacuo: 3-(5-hydroxypyrimidin-2-yl)benzoic acid as brownish crystals; m.p. 293-295°; ESI 217 (M+H); HPLC: Rt.=2.19 min (method A).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08877751B2uspto-grants-2014_11