Iodoethane → 2-chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine

HRID 9902

반응식

HRID 9902 반응식
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4]([NH:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=2)[N:3]=1.C(=O)([O-])[O-].[Cs+].[Cs+].[CH2:28](I)[CH3:29]>O1CCOCC1.O.CN(C=O)C.C(OCC)(=O)C>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:28][CH3:29])=[C:4]([NH:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:19])[F:20])[CH:13]=2)[N:3]=1

참가 물질

6

반응물 3

HCID 6340IodoethaneHCID 10796Cesium carbonateHCID 219882372-Chloro-6-(3-trifluoromethyl-phenyl-amino)-purine

생성물 1

HCID 219881872-chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 86622776DMF dioxane water용매

실험 절차

A mixture comprising 1 g (3.2 mmol) of 2-chloro-6-(3-trifluoromethyl-phenyl-amino)-purine, 1.7 g (5.1 mmol) of caesium carbonate and 2.1 ml (25.6 mmol) of ethyl iodide in 7 ml of dioxane/water/DMF (8:2:2) is stirred at RT for 18 h. It is then diluted with ethyl acetate and the organic phase is washed with water. This phase is separated off and dried over sodium sulfate. After removal of the solvent, the residue is recrystallized from ethyl acetate and diethyl ether. 2-Chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine is obtained; m.p. 129–130° C.; FAB-MS: (M+H)+=342; Rf=0.6 (methylene chloride:methanol=9:1).

후처리

  1. washthe organic phase is washed with water
  2. customThis phase is separated off
  3. dry with materialdried over sodium sulfate
  4. customAfter removal of the solvent
  5. customthe residue is recrystallized from ethyl acetate and diethyl ether

출처 및 근거

ORD 기록
ord-bf83831a158f40d799e226584860bcea
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091346B1

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