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

HRID 9902

反応式

HRID 9902 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 86622776DMF dioxane water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-bf83831a158f40d799e226584860bcea
出典データセット
uspto-grants-2006_08
特許番号
US07091346B1

関連ノート

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