Aluminium lithium hydride → HCID 67261360、化合物

HRID 79309

反応式

HRID 79309 の反応式
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([CH2:7][N:8]2[CH:12]=[C:11]([C:13](OCC)=[O:14])[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[CH:12]=[C:11]([CH2:13][OH:14])[CH:10]=[N:9]2)=[CH:18][CH:19]=1

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 44558860ethyl 1-(4-methoxybenzyl)-1H-pyrazole-4-carboxylate

生成物 1

HCID 67261360HCID 67261360、化合物収率 75.6%

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-4-carboxylate (8.31 g, 31.9 mmol) in THF (100 mL) at 0° C. was added lithium aluminum hydride (1.45 g, 38.3 mmol). The cold bath was removed and the reaction was stirred for 3 hours. The reaction mixture was diluted with Et2O (200 mL) and Celite (10 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, which was then filtered, and the filter pad was washed with EtOAc (100 mL) and concentrated to provide the desired product (5.26 g).

後処理

  1. customThe cold bath was removed
  2. additionThe reaction mixture was diluted with Et2O (200 mL) and Celite (10 g)
  3. additionwas added to the reaction mixture
  4. additionsodium sulfate decahydrate was cautiously added
  5. customto quench
  6. customthe reaction, which
  7. filtrationwas then filtered
  8. washthe filter pad was washed with EtOAc (100 mL)
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-a57c2180b57a44a2b6609ca0acbd1b6b
出典データセット
uspto-grants-2014_09
特許番号
US08841455B2

関連ノート

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