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Potassium Iodide → 3-[5-(2-chlorophenyl)-2-iodo-1,3-oxazol-4-yl]-4-{[2-(trimethylsilyl)-ethoxy]methyl}-4H-1,2,4-triazole

HRID 537047
ノート
印刷プレビュー

反応式

HRID 537047 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[O:12][C:11]([I:13])=[N:10][C:9]=1[C:14]1[N:18]=[CH:17][NH:16][N:15]=1.[CH3:19][Si:20]([CH2:23][CH2:24][O:25][CH2:26]Cl)([CH3:22])[CH3:21].[I-].[K+].[H-].[Na+]>CN(C=O)C.O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[O:12][C:11]([I:13])=[N:10][C:9]=1[C:14]1[N:18]([CH2:26][O:25][CH2:24][CH2:23][Si:20]([CH3:22])([CH3:21])[CH3:19])[CH:17]=[N:16][N:15]=1
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 4

HCID 4875Potassium IodideHCID 24758Sodium hydrideHCID 27242712-Chloromethyl 2-(trimethylsilyl)ethyl etherHCID 178478028HCID 178478028、化合物

生成物 1

HCID 667494963-[5-(2-chlorophenyl)-2-iodo-1,3-oxazol-4-yl]-4-{[2-(trimethylsilyl)-ethoxy]methyl}-4H-1,2,4-triazole収率 11.1%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒

実験手順

To a mixture of 3-[5-(2-chlorophenyl)-2-iodo-1,3-oxazol-4-yl]-1H-1,2,4-triazole (26.0 g, 70.0 mmol), SEM-Cl (16.6 g, 100.0 mmol) and potassium iodide (1.6 g, 10.0 mmol) in DMF (400 mL) was added NaH (4.0 g, 100 mmol). The reaction mixture was allowed to stir at rt until the reaction was complete (as judged by TLC analysis). The reaction mixture was poured into water and extracted with EtOAc. The organic solutions were combined, dried over MgSO4, filtered and concentrated. The residue was purified by column chromatography to give 3-[5-(2-chlorophenyl)-2-iodo-1,3-oxazol-4-yl]-4-{[2-(trimethylsilyl)-ethoxy]methyl}-4H-1,2,4-triazole (3.9 g, 11%) plus two other SEM regioisomers (9.39 g, 26.2%). All three isomers could be separated and could be used for the following steps.

後処理

  1. extractionextracted with EtOAc
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-68f56bad6e0b41bda031d113fc4d7a48
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08859768B2

反応ノート

読み込み中…

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