Water → (2-Methoxypyridin-4-yl)methanol

HRID 709750ノート

反応式

HRID 709750 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][C:9]1[CH:10]=[C:11]([CH:16]=[CH:17][N:18]=1)[C:12](OC)=[O:13].O.[OH-].[Na+]>C(OCC)C.C1COCC1>[CH3:7][O:8][C:9]1[CH:10]=[C:11]([CH2:12][OH:13])[CH:16]=[CH:17][N:18]=1

参加物

7

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 14223465Methyl 2-methoxyisonicotinateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 14462410(2-Methoxypyridin-4-yl)methanol収率 94.5%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

To a suspension of lithium aluminum hydride (2.92 g) in diethyl ether (200 ml) and THF (50 mL) was added dropwise a solution of methyl 2-methoxyisonicotinate (8.57 g) in diethyl ether (50 mL) at 0° C., and the reaction mixture was stirred at 0° C. for 20 min. Water (3.0 mL), 4N aqueous sodium hydroxide solution (3.0 mL) and water (9.0 mL) were successively added to the reaction mixture at 0° C., and the mixture was stirred at room temperature for 15 min. The resulting white precipitate was filtered off, and the solvent in the filtrate was evaporated under reduced pressure to give a crude product of the title compound (6.74 g) as a pale-yellow oil. This compound was used for the next step without further purification.

後処理

  1. stirringthe mixture was stirred at room temperature for 15 min
  2. filtrationThe resulting white precipitate was filtered off
  3. customthe solvent in the filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-0108bed5ea1344e6a251bc82f242eb61
出典データセット
uspto-grants-2015_11
特許番号
US09181186B2

反応ノート

読み込み中…