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

Trimethylsilyl triflate → 4,5-Dichloro-1-(2,3-di-O-acetyl-5-deoxy-beta-D-ribofuranosyl)-N-(1-methylethyl)-1H-benzimidazol-2-amine

HRID 2227178
ノート
印刷プレビュー

反応式

HRID 2227178 の反応式
[Cl:1][C:2]1[C:10]2[N:9]=[C:8]([NH:11][CH:12]([CH3:14])[CH3:13])[NH:7][C:6]=2[CH:5]=[CH:4][C:3]=1[Cl:15].C/C(/O[Si](C)(C)C)=N\[Si](C)(C)C.FC(F)(F)S(O[Si](C)(C)C)(=O)=O.C(O[CH:44]1[O:56][C@H:55]([CH3:57])[C@@H:50]([O:51][C:52](=[O:54])[CH3:53])[C@H:45]1[O:46][C:47](=[O:49])[CH3:48])(=O)C.C(=O)(O)[O-].[Na+]>C(#N)C>[Cl:1][C:2]1[C:10]2[N:9]=[C:8]([NH:11][CH:12]([CH3:13])[CH3:14])[N:7]([C@@H:44]3[O:56][C@H:55]([CH3:57])[C@@H:50]([O:51][C:52](=[O:54])[CH3:53])[C@H:45]3[O:46][C:47](=[O:49])[CH3:48])[C:6]=2[CH:5]=[CH:4][C:3]=1[Cl:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 65367Trimethylsilyl triflateHCID 516892Sodium BicarbonateHCID 6913588N,O-bis(trimethylsilyl)acetamideHCID 11196237Tri-O-acetyl-5-deoxy-D-ribofuranoseHCID 184219284,5-Dichloro-N-(1-methylethyl)-1H-benzimidazol-2-amine

生成物 1

HCID 57052773
4,5-Dichloro-1-(2,3-di-O-acetyl-5-deoxy-beta-D-ribofuranosyl)-N-(1-methylethyl)-1H-benzimidazol-2-amine
収率 90%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

4,5-Dichloro-N-(1-methylethyl)-1H-benzimidazol-2-amine (0.50 g, 2.0 mmol), N,O-bis(trimethylsilyl) acetamide (Aldrich, 0.55 mL, 2.2 mmol), and acetonitrile (Aldrich Sure Seal, 70 mL) were combined and refluxed under nitrogen for 15 min. The solution was cooled to rt and trimethylsilyl trifluoromethanesulfonate (Aldrich, 0.24 mL, 1.2 mmol) was added. After 10 min, 1,2,3-tri-O-acetyl-5-deoxy-D-ribofuranose (0.69 g, 2.6 mmol) dissolved in acetonitrile (Aldrich Sure Seal, 10 mL) was added. The solution was stirred under nitrogen at rt for 12 h and then heated in an 80° C. oil bath for 2.5 h. The solution was then poured into 5% aqueous sodium bicarbonate (50 mL) and extracted with ethyl acetate (3×100 mL). The organic layers were dried with magnesium sulfate, filtered, and evaporated. The crude residue was purified on a silica gel column (2.5×20 cm, 230-400 mesh) with 97:3 dichloromethane-methanol to give the title compound (0.82 g, 1.8 mmol, 90%); 1H NMR (DMSO-d6) δ: 7.29 (s, 1H, Ar—H, J=8.4 Hz), 7.10 (s, 1H, Ar—H, J=8.4 Hz), 6.98 (d, 1H, NH, J=7.5 Hz), 6.10 (d, 1H, H-1′, J=6.3 Hz), 5.50-5.55 (m, 1H, CH), 5.15 (t, 1H, CH, J=6.0 Hz), 4.04-4.17 (m, 2H, CH), 2.14 (s, 3H, OAc), 2.01 (s, 3H, OAc), 1.48 (d, 3H, 5′-CH3, J=6.3 Hz), 1.24 (t, 6H, CH3, J=6.2 Hz).

後処理

  1. temperaturerefluxed under nitrogen for 15 min
  2. additionwas added
  3. temperatureheated in an 80° C. oil bath for 2.5 h
  4. extractionextracted with ethyl acetate (3×100 mL)
  5. dry with materialThe organic layers were dried with magnesium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. customThe crude residue was purified on a silica gel column (2.5×20 cm, 230-400 mesh) with 97:3 dichloromethane-methanol

出典と根拠

ORDレコード
ord-205a0cdac3334cee9212788e51bc6ab0
出典データセット
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06413938B1

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