反应 #40359

ord-5891a95dbe0a4f5487ba99d0197a9015

反应方程式

CCNC
methyl ethyl amine
Cc1cc(Oc2ccnc(N(C)c3ccccc3)n2)c(C)cc1N
[4-(4-Amino-2,5-dimethyl-phenoxy)-pyrimidin-2-yl]-methyl-phenyl-amine
COC(OC)OC
trimethoxymethane
Cc1ccc(S(=O)(=O)O)cc1
p-toluene sulfonic acid
CCN(C)C=Nc1cc(C)c(Oc2ccnc(N(C)c3ccccc3)n2)cc1C
N′-{2,5-dimethyl-4-[2-(methyl-phenyl-amino)-pyrimidin-4-yloxy]-phenyl}-N-ethyl-N-methyl-formamidine

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwere added
  2. 2
    温度The reaction mixture was refluxed for 2 hrs
  3. 3
    浓缩concentrated in vacuo
  4. 4
    其他was evaporated
  5. 5
    其他yielded 280 mg (89%) with a purity of 87%

实验过程

To a mixture of 252 mg (0.7 mmol) of [4-(4-Amino-2,5-dimethyl-phenoxy)-pyrimidin-2-yl]-methyl-phenyl-amine and 4 ml of trimethoxymethane, 20 mg of p-toluene sulfonic acid were added. The reaction mixture was refluxed for 2 hrs and concentrated in vacuo. The mixture was solved in 10 ml of dichloromethane and 62 mg (1.05 mmol) methyl ethyl amine was added. After stirring 18 hrs at ambient temperature the mixture was evaporated and yielded 280 mg (89%) with a purity of 87%; log P (pH 2.3)=1.61.

来源

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