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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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4-Toluenesulfonyl chloride → 5'-Azidoguanosine

HRID 847441
ノート
印刷プレビュー

反応式

HRID 847441 の反応式
NC[C@H]1O[C@@H](N2C3N=C(N)NC(=O)C=3N=C2)C[C@@H]1O.[C@@H:20]1([N:28]2[C:38]3[N:37]=[C:35]([NH2:36])[NH:34][C:32](=[O:33])[C:31]=3[N:30]=[CH:29]2)[O:27][C@H:24]([CH2:25][OH:26])[C@@H:22]([OH:23])[CH2:21]1.S(Cl)(C1C=CC(C)=CC=1)(=O)=O.S(C1C=CC(C)=CC=1)([O-])(=O)=[O:51].[N-:61]=[N+:62]=[N-:63].[Na+]>N1C=CC=CC=1.CN(C=O)C>[N:61]([CH:25]([OH:26])[C@H:24]1[O:27][C@@H:20]([N:28]2[C:38]3[N:37]=[C:35]([NH2:36])[NH:34][C:32](=[O:33])[C:31]=3[N:30]=[CH:29]2)[C@H:21]([OH:51])[C@@H:22]1[OH:23])=[N+:62]=[N-:63]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 73974-Toluenesulfonyl chlorideHCID 33557Sodium AzideHCID 85570p-ToluenesulfonateHCID 135398592DeoxyguanosineHCID 1358167395'-Amino-2',5'-dideoxyguanosine

生成物 1

HCID 1364033885'-Azidoguanosine

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒
HCID 6228Dimethylformamide溶媒

実験手順

An alternate preparation of 5'-amino-2',5'-dideoxyguanosine is to treat the protected 2'-deoxyguanosine (protected at either the N-2-phenylacetyl or the N-2-FMOC derivative) (1 mmol) with tosyl chloride (1.3 mmol) in pyridine at 0° C. overnight. The solution is evaporated to dryness and the residue is dissolved in chloroform. The resulting solution is washed twice with aqueous sodium bicarbonate and dried over sodium sulfate. The solvent is evaporated and the residue chromatographed on silica gel eluting with methanol/chloroform mixtures. The resulting tosylate (1 mmol) is treated with sodium azide (6 mmol) in DMF at 80°-100° C. for a few h. The solvent is removed by rotovap and the residue is chromatographed on silica gel eluting with chloroform/ methanol solvent mixtures. The azide is reduced to the desired amine using the catalytic hydrogenation procedure above.

後処理

  1. customat 0° C.
  2. customovernight
  3. customThe solution is evaporated to dryness
  4. dissolutionthe residue is dissolved in chloroform
  5. washThe resulting solution is washed twice with aqueous sodium bicarbonate
  6. dry with materialdried over sodium sulfate
  7. customThe solvent is evaporated
  8. customthe residue chromatographed on silica gel eluting with methanol/chloroform mixtures
  9. customThe solvent is removed by rotovap
  10. customthe residue is chromatographed on silica gel eluting with chloroform/ methanol solvent mixtures

出典と根拠

ORDレコード
ord-a4b982b8ea954efdb3653c8c755cbf28
出典データセット
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05142047

反応ノート

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