Aluminium lithium hydride → HCID 67409860、化合物

HRID 1897523ノート

反応式

HRID 1897523 の反応式
[Si:1]([O:8][C:9]([CH3:31])([CH3:30])[CH2:10][N:11]1[C:19]2[C:14](=[CH:15][C:16]([O:20][C:21]3[CH:28]=[CH:27][C:26]([F:29])=[CH:25][C:22]=3[C:23]#[N:24])=[CH:17][CH:18]=2)[CH:13]=[N:12]1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[Si:1]([O:8][C:9]([CH3:31])([CH3:30])[CH2:10][N:11]1[C:19]2[C:14](=[CH:15][C:16]([O:20][C:21]3[CH:28]=[CH:27][C:26]([F:29])=[CH:25][C:22]=3[CH2:23][NH2:24])=[CH:17][CH:18]=2)[CH:13]=[N:12]1)([C:4]([CH3:7])([CH3:5])[CH3:6])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 674118002-{1-[2-(tert-butyldimethylsilanyloxy)-2-methyl-propyl]-1H-indazol-5-yloxy}-5-fluorobenzonitrile

生成物 1

HCID 67409860HCID 67409860、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a cooled (0° C.) solution of 2-{1-[2-(tert-butyldimethylsilanyloxy)-2-methyl-propyl]-1H-indazol-5-yloxy}-5-fluorobenzonitrile (0.071 g, 0.162 mmol) in THF (2 mL) was added LAH (0.32 mL of 1M in THF). The solution was warmed to room temperature and stirred for 1 hour. The reaction mixture was cooled to 0° C. and quenched with water (12 μL), 3N NaOH (12 μL) and water (36 μL). The salts were removed by filtration and the filtrate was concentrated under reduced pressure and used in the next reaction without further purification.

後処理

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. customquenched with water (12 μL), 3N NaOH (12 μL) and water (36 μL)
  3. customThe salts were removed by filtration
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customused in the next reaction without further purification

出典と根拠

ORDレコード
ord-101c76ee150f4ba3ac63a9635288977c
出典データセット
uspto-grants-2013_08
特許番号
US08518983B2

反応ノート

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