Sodium citrate, potassium citrate, citric acid → 4-azidoacetyl-1-(2-deoxy-2-fluoro-beta-D-arabinofuranosyl)-5-(dimethylaminomethyleneamino)imidazole

HRID 1419487노트

반응식

HRID 1419487 반응식
C([O:4][C@@H:5]1[C@@H:9]([CH2:10][O:11]C(=O)C)[O:8][C@@H:7]([N:15]2[C:19]([N:20]=[CH:21][N:22]([CH3:24])[CH3:23])=[C:18]([C:25](=[O:30])[CH2:26][N:27]=[N+:28]=[N-:29])[N:17]=[CH:16]2)[C@H:6]1[F:31])(=O)C.C[O-].[Na+].C(C(O)(C([O-])=O)CC([O-])=O)C([O-])=O.C(C(O)(C([O-])=O)CC([O-])=O)C([O-])=O.O.[Na+].[Na+].[Na+].[K+].[K+].[K+]>CO>[N:27]([CH2:26][C:25]([C:18]1[N:17]=[CH:16][N:15]([C@@H:7]2[O:8][C@H:9]([CH2:10][OH:11])[C@@H:5]([OH:4])[C@@H:6]2[F:31])[C:19]=1[N:20]=[CH:21][N:22]([CH3:24])[CH3:23])=[O:30])=[N+:28]=[N-:29]

참가 물질

5

반응물 3

HCID 171403Sodium citrate, potassium citrate, citric acidHCID 10942334Sodium MethoxideHCID 542783091-(3,5-di-O-acetyl-2-deoxy-2-fluoro-beta-D-arabinofuranosyl)-4-azidoacetyl-5-(dimethylaminomethyleneamino) imidazole

생성물 1

HCID 544024694-azidoacetyl-1-(2-deoxy-2-fluoro-beta-D-arabinofuranosyl)-5-(dimethylaminomethyleneamino)imidazole수율 77%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

Compound (39) (50 mg) obtained in item (6) above was dissolved in methanol (2 ml), to which was then added a 0.2M sodium methylate solution (0.2 ml) in methanol. The mixture obtained was allowed to undergo the reaction at room temperature for 20 minutes. The resulting reaction solution was neutralized with addition of ion-exchange resin, Amberlite CG-120 (H+ form) (100-200 mesh) and filtered, and the filtrate was concentrated. The solid residue obtained was washed with diethylether to give the titled compound (40) (31 mg) as an insoluble solid. Yield: 77%.

후처리

  1. customThe mixture obtained
  2. customthe reaction at room temperature for 20 minutes
  3. customThe resulting reaction solution
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated
  6. customThe solid residue obtained
  7. washwas washed with diethylether

출처 및 근거

ORD 기록
ord-1007395822e147008e9c30a74abacbfd
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05886167

반응 노트

불러오는 중…