Aluminium lithium hydride → HCID 66959407、化合物

HRID 1958861ノート

反応式

HRID 1958861 の反応式
[CH3:1][C:2]1[CH:19]=[CH:18][CH:17]=[C:16]([CH3:20])[C:3]=1[CH2:4][O:5][C:6]1[C:7]([O:14][CH3:15])=[C:8]([CH:11]=[CH:12][CH:13]=1)[CH:9]=[O:10].[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[CH3:1][C:2]1[CH:19]=[CH:18][CH:17]=[C:16]([CH3:20])[C:3]=1[CH2:4][O:5][C:6]1[C:7]([O:14][CH3:15])=[C:8]([CH2:9][OH:10])[CH:11]=[CH:12][CH:13]=1

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 866570083-(2,6-Dimethylbenzyloxy)-2-methoxybenzaldehyde

生成物 1

HCID 66959407HCID 66959407、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 3-(2,6-Dimethylbenzyloxy)-2-methoxybenzaldehyde (Step B, 10.6 g, 32.7 mmol) in dry THF (40 ml) was added drop wise LiAlH4 (1M in THF, 0.95 g, 23.7 mmol) at 0° C. under argon. The reaction mixture was stirred for 1 hours or until all the starting material is consumed, then quenched by adding water slowly, followed by addition of 1N HCl (5 ml), water (10 ml), and EtOAc (20 ml) was added to the reaction mixture. The reaction mixture was concentrated, and passed through a short silica gel column using ethyl acetate to give the title compound as an off white solid.

後処理

  1. customis consumed
  2. customquenched
  3. additionby adding water slowly
  4. additionfollowed by addition of 1N HCl (5 ml), water (10 ml), and EtOAc (20 ml)
  5. additionwas added to the reaction mixture
  6. concentrationThe reaction mixture was concentrated

出典と根拠

ORDレコード
ord-f117fc55acda429b91553d365c579183
出典データセット
uspto-grants-2013_04
特許番号
US08410154B2

反応ノート

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