반응식
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4]([Cl:11])[N:3]=1.[H-].[Na+].[H][H].[CH:16](I)([CH3:18])[CH3:17]>CN(C=O)C>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH:16]([CH3:18])[CH3:17])=[C:4]([Cl:11])[N:3]=1참가 물질
실험 절차
To a solution of 0.67 g of 2,6-dichloropurine in 5 mL of dry DMF at room temperature was added 0.16 gms (1.1 eq.) of 50% sodium hydride/oil powder.Upon cessation of hydrogen evolution, a large excess (2 mL) of isopropyl iodide was added to the anionic solution. This reaction solution was stirred for three days at ambient temperature. The reaction was quenched with 30 mL of water and extracted with ethyl acetate (3×50 mL). The organic extracts were combined and back washed with 3×50 mL of waterfollowed by 20 mL of brine. The ethyl acetate solution was dried over anhydrous magnesium sulfate and evaporated. The compound was subjected to variable gradient flash chromatography on silica gel with hexane/ethyl acetate mixtures and yielded 0.37 gms of desired N-9 product (45%) and 0.08 gms of the N-7 isomer(10%).
후처리
- customThe reaction was quenched with 30 mL of water
- extractionextracted with ethyl acetate (3×50 mL)
- washback washed with 3×50 mL of waterfollowed by 20 mL of brine
- dry with materialThe ethyl acetate solution was dried over anhydrous magnesium sulfate
- customevaporated
출처 및 근거
- ORD 기록
- ord-9a0d011c5c81437dbbce13410c0cc588
- 출처 데이터셋
- uspto-grants-1999_02
- 특허 번호
- US05866702
연결된 노트
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