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Aluminium lithium hydride → HCID 67259679、化合物

HRID 79339
ノート
印刷プレビュー

反応式

HRID 79339 の反応式
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([CH2:7][N:8]2[C:12]([C:13](OCC)=[O:14])=[CH:11][CH:10]=[N:9]2)=[CH:5][CH:4]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][N:8]2[C:12]([CH2:13][OH:14])=[CH:11][CH:10]=[N:9]2)=[CH:18][CH:19]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 54208979ethyl 1-(4-methoxybenzyl)-1H-pyrazole-5-carboxylate

生成物 1

HCID 67259679HCID 67259679、化合物収率 89.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

To ethyl 1-(4-methoxybenzyl)-1H-pyrazole-5-carboxylate (1.81 g, 6.95 mmol) in THF (20 mL) at 0° C. was added lithium aluminum hydride (0.317 g, 8.34 mmol). The cold bath was removed. The reaction mixture was stirred for 5 hours, diluted with Et2O (50 mL) and Celite (5 g) was added to the reaction mixture. The mixture was cooled to 0° C. and sodium sulfate decahydrate was cautiously added to quench the reaction. The mixture was filtered and washed with EtOAc (100 mL). The solution was concentrated under reduced pressure to give the product (1.36 g).

後処理

  1. customThe cold bath was removed
  2. additiondiluted with Et2O (50 mL) and Celite (5 g)
  3. additionwas added to the reaction mixture
  4. additionsodium sulfate decahydrate was cautiously added
  5. customto quench
  6. customthe reaction
  7. filtrationThe mixture was filtered
  8. washwashed with EtOAc (100 mL)
  9. concentrationThe solution was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-e63722a65ef64491b462ae6f320ce308
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08841455B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート