反应 #40364

ord-7ccb126b89ca40838648d5c99efc243b

反应方程式

Cc1cc(Oc2cc(C)c(N)cc2C)nc(Cl)n1
4-[(2-chloro-6-methylpyrimidin-4-yl)oxy]-2,5-dimethyl-aniline
CC#N
acetonitrile
CCN(C)C(OC)OC
N-(dimethoxymethyl)-N-methylethanamine
CCN(C)C=Nc1cc(C)c(Oc2cc(C)nc(Cl)n2)cc1C
N′-{4-[(2-chloro-6-methylpyrimidin-4-yl)oxy]-2,5-dimethylphenyl}-N-ethyl-N-methylimido-formamide

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwas added
  2. 2
    温度The reaction mixture was refluxed for 20 hrs
  3. 3
    浓缩The reaction mixture was concentrated in vacuo
  4. 4
    workup.ADDITIONdiluted with ethyl acetate
  5. 5
    洗涤washed with water
  6. 6
    干燥The organic layer was dried over magnesium sulfate
  7. 7
    浓缩concentrated in vacuo
  8. 8
    其他yielded 220 mg (59%) with a purity of 72% log P (pH=2.3)=1.45

实验过程

To a mixture of 310 mg (0.8 mmol) of 4-[(2-chloro-6-methylpyrimidin-4-yl)oxy]-2,5-dimethyl-aniline in 20 ml acetonitrile 208 mg (1.5 mmol) of N-(dimethoxymethyl)-N-methylethanamine (77% pure) was added. The reaction mixture was refluxed for 20 hrs. The reaction mixture was concentrated in vacuo, diluted with ethyl acetate and washed with water. The organic layer was dried over magnesium sulfate and concentrated in vacuo yielded 220 mg (59%) with a purity of 72% log P (pH=2.3)=1.45.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07727986B2uspto-grants-2010_06