Water → 9-((2-Acetoxyethoxy)methyl)-6-chloropurine

HRID 892350

반응식

HRID 892350 반응식
[Cl:1][C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[NH:4][CH:5]=[N:6]2.[H-].[Na+].[C:13]([O:16][CH2:17][CH2:18][O:19][CH2:20]Br)(=[O:15])[CH3:14].O>CN(C=O)C>[C:13]([O:16][CH2:17][CH2:18][O:19][CH2:20][N:6]1[CH:5]=[N:4][C:3]2[C:7]1=[N:8][CH:9]=[N:10][C:2]=2[Cl:1])(=[O:15])[CH3:14]

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 3676562-(Bromomethoxy)ethyl acetateHCID 53592776-Chloropurine

생성물 1

HCID 5126559-((2-Acetoxyethoxy)methyl)-6-chloropurine수율 68%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 6-chloropurine (6 g, 38.8 mmoles) in DMF was added sodium hydride 60% (0.93 g) over 1.5 hour period. (2-acetoxyethoxy)methyl bromide was then added at room temperature; the reaction mixture was allowed to stir for 2 hours under Nz atmosphere. H2O was added and the product was extracted with ethyl acetate. The organic phase was dried over MgSO4, filtered, and evaporated in vacuo to give a light yellow solid 7.1 g, 68% yield of 9-[(2-acetoxy-ethoxy)methyl]-6-chloro-purine. The crude was used without further purification.

후처리

  1. extractionthe product was extracted with ethyl acetate
  2. dry with materialThe organic phase was dried over MgSO4
  3. filtrationfiltered
  4. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-f44e10d4426d48e2be129f56c37ce4e1
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05117830

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