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Sodium sulfate decahydrate → (1-(4-methoxybenzyl)-1H-1,2,3-triazol-4-yl)methanol

HRID 1171747
ノート
印刷プレビュー

反応式

HRID 1171747 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][C:9]1[CH:25]=[CH:24][C:12]([CH2:13][N:14]2[CH:18]=[C:17]([C:19](OCC)=[O:20])[N:16]=[N:15]2)=[CH:11][CH:10]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:7][O:8][C:9]1[CH:10]=[CH:11][C:12]([CH2:13][N:14]2[CH:18]=[C:17]([CH2:19][OH:20])[N:16]=[N:15]2)=[CH:24][CH:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 12937510Ethyl 1-(4-methoxybenzyl)-1H-1,2,3-triazole-4-carboxylateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 23139019(1-(4-methoxybenzyl)-1H-1,2,3-triazol-4-yl)methanol収率 94.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To tetrahydrofuran (THF, 500 ml) was added carefully lithium aluminium hydride (7.3 g) with stirring. The resulting mixture was stirred at 0° C., to which was added dropwise a solution of ethyl 1-(4-methoxybenzyl)-1H-1,2,3-triazole-4-carboxylate (50.0 g) in THF (500 ml). The resulting mixture was stirred at room temperature for 30 minutes, and the reaction was stopped by careful addition of sodium sulfate decahydrate. The slurry mixture was stirred at room temperature for 2 hours further, filtered to remove solids, and the filtrate was concentrated in vacuo to afford [1-(4-methoxybenzyl)-1H-1,2,3-triazol-4-yl]methanol (39.51 g, yield: 94%).

後処理

  1. stirringThe resulting mixture was stirred at 0° C., to which
  2. stirringThe resulting mixture was stirred at room temperature for 30 minutes
  3. stirringThe slurry mixture was stirred at room temperature for 2 hours further
  4. filtrationfiltered
  5. customto remove solids
  6. concentrationthe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-0e24035e59704a1cb6a00b653555bfbb
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07829580B2

反応ノート

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