Cesium carbonate → HCID 59395867, 화합물

HRID 1097646

반응식

HRID 1097646 반응식
[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

참가 물질

5

반응물 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

생성물 1

HCID 59395867HCID 59395867, 화합물수율 75%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-25feb408d3cd4f77addbaeeb92f4cebe
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143264B2

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