Azobisisobutyronitrile → 1-[5-O-(t-butyldiphenylsilyl)-2,3-dideoxy-2,2-di(phenylthio)-alpha-D-glycero-pentofuranosyl]uracil

HRID 36759ノート

反応式

HRID 36759 の反応式
[Si:1]([O:18][CH2:19][C@H:20]1[O:24][C@@H:23]([N:25]2[CH:32]=[CH:31][C:29](=[O:30])[NH:28][C:26]2=[O:27])[C:22]([S:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)([S:33][C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[CH2:21]1)([C:14]([CH3:17])([CH3:16])[CH3:15])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC(N=NC(C#N)(C)C)(C#N)C>C1C=CC=CC=1>[Si:1]([O:18][CH2:19][C@H:20]1[O:24][C@H:23]([N:25]2[CH:32]=[CH:31][C:29](=[O:30])[NH:28][C:26]2=[O:27])[C:22]([S:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)([S:33][C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[CH2:21]1)([C:14]([CH3:15])([CH3:16])[CH3:17])([C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参加物

4

反応物 2

HCID 6547AzobisisobutyronitrileHCID 111150361-[5-O-(t-butyldiphenylsilyl)-2,3-dideoxy-2,2-di(phenylthio)-beta-D-glycero-pentofuranosyl]uracil

生成物 1

HCID 152169961-[5-O-(t-butyldiphenylsilyl)-2,3-dideoxy-2,2-di(phenylthio)-alpha-D-glycero-pentofuranosyl]uracil

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To a solution prepared by dissolving 7 mg (0.10 mmol) of 1-[5-O-(t-butyldiphenylsilyl)-2,3-dideoxy-2,2-di(phenylthio)-β-D-glycero-pentofuranosyl]uracil prepared in step (3) in 10 ml of anhydrous benzene, 150 μl (0.57 mmol) of hydrogenated tributyl tin and 10 mg of azobisisobutylonitrile were added, followed by subjecting the resultant solution to a reflux under heating for 48 hours under an argon gas atmosphere. After completion of the reaction, a low boiling point substances were removed by distillation under a reduced pressure so as to obtain a residue.

後処理

  1. customTo a solution prepared
  2. additionwere added
  3. temperaturea reflux
  4. temperatureunder heating for 48 hours under an argon gas atmosphere
  5. customAfter completion of the reaction
  6. customa low boiling point substances were removed by distillation under a reduced pressure so as
  7. customto obtain a residue

出典と根拠

ORDレコード
ord-f798647032db4cd8b9a00f3604fcfd6d
出典データセット
uspto-grants-1995_05
特許番号
US05416204

反応ノート

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