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Aluminium lithium hydride → HCID 86625534、化合物

HRID 2266021
ノート
印刷プレビュー

反応式

HRID 2266021 の反応式
[CH2:1]([C:3]1[N:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:12]=[CH:11][C:4]=1[C:5](N(OC)C)=[O:6])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[CH2:1]([C:3]1[C:4]([CH:5]=[O:6])=[CH:11][CH:12]=[C:13]([C:15]([F:18])([F:16])[F:17])[N:14]=1)[CH3:2]
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 59598165HCID 59598165、化合物

生成物 1

HCID 86625534HCID 86625534、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-10 °C

実験手順

To a cooled (−78° C.) solution of 2-ethyl-N-methoxy-N-methyl-6-trifluoromethyl-nicotinamide (113 mg, 0.43 mmol) in THF (4 mL) was added lithium aluminum hydride (1M LAH in THF, 0.22 mL). The mixture was stirred for 15 minutes, and then warmed to −10° C. After additional stirring for 30 minutes, the mixture was quenched with saturated potassium hydrogen sulfate solution (1 mL) and extracted with diethyl ether. The organic layer was dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure to give 2-ethyl-6-trifluoromethyl-pyridine-3-carbaldehyde quantitatively as oil. The crude product was used directly in the following reaction.

後処理

  1. stirringAfter additional stirring for 30 minutes
  2. customthe mixture was quenched with saturated potassium hydrogen sulfate solution (1 mL)
  3. extractionextracted with diethyl ether
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-c09692f65bac4c1ebd966a2df79f3777
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07858621B2

反応ノート

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