Sodium Carbonate → HCID 59299588, 화합물

HRID 1097647

반응식

HRID 1097647 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])[NH:5][C:4]=2[N:3]=1.C(=O)([O-])[O-].[Na+].[Na+].Br[CH2:23][CH2:24][CH2:25][C:26]([F:29])([F:28])[F:27]>CN(C=O)C>[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]([CH2:23][CH2:24][CH2:25][C:26]([F:29])([F:28])[F:27])[C:4]=2[N:3]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 5210064-Bromo-1,1,1-trifluorobutaneHCID 592995327-Allyl-8-chloro-1H-purine-2,6(3H,7H)-dione

생성물 1

HCID 59299588HCID 59299588, 화합물수율 40%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

A solution of 8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (2.0 g, 8.8 mmol) in DMF (20 ml) was treated with sodium carbonate (1.15 g, 10.8 mmol) and 4-bromo-1,1,1-trifluorobutane (1.86 g, 9.7 mmol). The mixture was stirred at 50° C. for 18 h then cooled and evaporated. The residue was partitioned between EtOAc (100 ml) and saturated aqueous sodium bicarbonate (50 ml). The organic phase was dried (MgSO4), filtered and evaporated. The residue was triturated in a mixture of diethyl ether and cyclohexane then the product filtered off and dried to yield the title compound as a white solid (1.18 g, 40%).

후처리

  1. temperaturethen cooled
  2. customevaporated
  3. customThe residue was partitioned between EtOAc (100 ml) and saturated aqueous sodium bicarbonate (50 ml)
  4. dry with materialThe organic phase was dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was triturated in a mixture of diethyl ether and cyclohexane
  8. filtrationthe product filtered off
  9. customdried

출처 및 근거

ORD 기록
ord-9da0aabc817a471d9ca88ff34cc418da
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143264B2

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