ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
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
  1. ホーム
  2. /反応

4-Toluenesulfonyl chloride → 5'-Azidoguanosine

HRID 1587279
ノート
印刷プレビュー

反応式

HRID 1587279 の反応式
NC[C@H]1O[C@@H](N2C3N=C(N)NC(=O)C=3N=C2)C[C@@H]1O.NC[C@H]1O[C@@H](N2C3N=CN=C(O)C=3N=C2)C[C@@H]1O.[C@@H:38]1([N:46]2[C:56]3[N:55]=[C:53]([NH2:54])[NH:52][C:50](=[O:51])[C:49]=3[N:48]=[CH:47]2)[O:45][C@H:42]([CH2:43][OH:44])[C@@H:40]([OH:41])[CH2:39]1.S(Cl)(C1C=CC(C)=CC=1)(=O)=O.S(C1C=CC(C)=CC=1)([O-])(=O)=[O:69].[N-:79]=[N+:80]=[N-:81].[Na+].[N-]=[N+]=[N-].[Li+]>N1C=CC=CC=1.CN(C=O)C>[N:79]([CH:43]([OH:44])[C@H:42]1[O:45][C@@H:38]([N:46]2[C:56]3[N:55]=[C:53]([NH2:54])[NH:52][C:50](=[O:51])[C:49]=3[N:48]=[CH:47]2)[C@H:39]([OH:69])[C@@H:40]1[OH:41])=[N+:80]=[N-:81]
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 7

HCID 73974-Toluenesulfonyl chlorideHCID 33557Sodium AzideHCID 85570p-ToluenesulfonateHCID 88163Lithium azideHCID 135398592DeoxyguanosineHCID 1358167395'-Amino-2',5'-dideoxyguanosineHCID 178511304HCID 178511304、化合物

生成物 1

HCID 1364033885'-Azidoguanosine

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6228Dimethylformamide溶媒2 回

実験手順

An alternate preparation of 5'-amino-2',5'-dideoxyguanosine (or 5'-amino-2',5'-dideoxyinosine) is to treat the protected 2'-deoxy guanosine (protected as the N-2-acetyl, 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, or lithium azide (10 mmol) in DMF at 60° C. for several 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 above procedure.

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-6b015f7e053948508d21916e286e2077
出典データセット
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05217866

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート