Cesium carbonate → HCID 59395867、化合物

HRID 1097646

反応式

HRID 1097646 の反応式
[Cl:1][C:2]1[N:10]([CH2:11][CH:12]=[CH2:13])[C:9]2[C:8](=[O:14])[NH:7][C:6](=[O:15])[N:5]([CH2:16][CH2:17][CH2:18][C:19]([F:22])([F:21])[F:20])[C:4]=2[N:3]=1.C(=O)([O-])[O-].[Cs+].[Cs+].Br[CH2:30][CH2:31][CH2:32][OH:33]>CN(C=O)C>[Cl:1][C:2]1[N:10]([CH2:11][CH:12]=[CH2:13])[C:9]2[C:8](=[O:14])[N:7]([CH2:30][CH2:31][CH2:32][OH:33])[C:6](=[O:15])[N:5]([CH2:16][CH2:17][CH2:18][C:19]([F:22])([F:20])[F:21])[C:4]=2[N:3]=1

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 123083-Bromo-1-propanolHCID 592995888-chloro-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione

生成物 1

HCID 59395867HCID 59395867、化合物収率 75%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

A solution of 8-chloro-7-(2-propen-1-yl)-3-(4,4,4-trifluorobutyl)-3,7-dihydro-1H-purine-2,6-dione (1.0 g, 3.0 mmol) in DMF (15 ml) was treated with caesium carbonate (1.16 g, 3.6 mmol) and 3-bromo-1-propanol (0.3 ml, 3.3 mmol). The mixture was heated at 60° C. for 4 h and then cooled and evaporated. The residue was partitioned between EtOAc (50 ml) and water (50 ml). The organic phase was dried (MgSO4), filtered and evaporated. The product was purified by flash chromatography using a gradient elution from cyclohexane to EtOAc. Product-containing fractions were combined and evaporated to give the title compound as a colourless oil (0.82 g, 75%).

後処理

  1. temperaturecooled
  2. customevaporated
  3. customThe residue was partitioned between EtOAc (50 ml) and water (50 ml)
  4. dry with materialThe organic phase was dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated
  7. customThe product was purified by flash chromatography
  8. washa gradient elution from cyclohexane to EtOAc
  9. customevaporated

出典と根拠

ORDレコード
ord-25feb408d3cd4f77addbaeeb92f4cebe
出典データセット
uspto-grants-2012_03
特許番号
US08143264B2

関連ノート

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