Sodium Azide → 7-(2-Azido-ethoxy)-1-(3-chloro-benzyl)-5-fluoro-3-(naphthalene-1-sulfonyl)-1H-indazole

HRID 2240060ノート

反応式

HRID 2240060 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:33]=[CH:34][CH:35]=1)[CH2:5][N:6]1[C:14]2[C:9](=[CH:10][C:11]([F:19])=[CH:12][C:13]=2[O:15][CH2:16][CH2:17]Cl)[C:8]([S:20]([C:23]2[C:32]3[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=3)[CH:26]=[CH:25][CH:24]=2)(=[O:22])=[O:21])=[N:7]1.[N-:36]=[N+:37]=[N-:38].[Na+]>CS(C)=O.O>[N:36]([CH2:17][CH2:16][O:15][C:13]1[CH:12]=[C:11]([F:19])[CH:10]=[C:9]2[C:14]=1[N:6]([CH2:5][C:4]1[CH:33]=[CH:34][CH:35]=[C:2]([Cl:1])[CH:3]=1)[N:7]=[C:8]2[S:20]([C:23]1[C:32]2[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=2)[CH:26]=[CH:25][CH:24]=1)(=[O:21])=[O:22])=[N+:37]=[N-:38]

参加物

5

反応物 2

HCID 33557Sodium AzideHCID 588121191-(3-Chloro-benzyl)-7-(2-chloro-ethoxy)-5-fluoro-3-(naphthalene-1-sulfonyl)-1H-indazole

生成物 1

HCID 866107637-(2-Azido-ethoxy)-1-(3-chloro-benzyl)-5-fluoro-3-(naphthalene-1-sulfonyl)-1H-indazole

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

A mixture of 1-(3-chloro-benzyl)-7-(2-chloro-ethoxy)-5-fluoro-3-(naphthalene -1-sulfonyl)-1H-indazole (0.1 g, 0.19 mmoles) and sodium azide (0.014 g, 0.22 mmoles) in DMSO (3 mL) was stirred together in a round bottom flask under nitrogen at 90° C. for 3 hours. Reaction mixture was cooled to room temperature, diluted with water, extracted with EtOAC, washed with water (2×), brine (1×), dried over Na2SO4, and concentrated under vacuum to afford the title compound as an off white solid (0.09 g, 0.17 mmoles).

後処理

  1. customReaction mixture
  2. temperaturewas cooled to room temperature
  3. extractionextracted with EtOAC
  4. washwashed with water (2×), brine (1×)
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-f63e95884ceb4480b6ded01e3aee5098
出典データセット
uspto-grants-2010_05
特許番号
US07723329B2

反応ノート

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