반응 #40359

ord-5891a95dbe0a4f5487ba99d0197a9015

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwere added
  2. 2
    온도The reaction mixture was refluxed for 2 hrs
  3. 3
    농축concentrated in vacuo
  4. 4
    기타was evaporated
  5. 5
    기타yielded 280 mg (89%) with a purity of 87%

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07727986B2uspto-grants-2010_06