Sodium sulfate decahydrate → (2-Methoxy-6-methylpyridin-3-yl)methanol

HRID 79273ノート

反応式

HRID 79273 の反応式
[CH3:1][O:2][C:3]1[N:12]=[C:11]([CH3:13])[CH:10]=[CH:9][C:4]=1[C:5](OC)=[O:6].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:1][O:2][C:3]1[C:4]([CH2:5][OH:6])=[CH:9][CH:10]=[C:11]([CH3:13])[N:12]=1

参加物

5

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 10910170METHYL 2-METHOXY-6-METHYLPYRIDINE-3-CARBOXYLATEHCID 21226445Aluminium lithium hydride

生成物 1

HCID 22678477(2-Methoxy-6-methylpyridin-3-yl)methanol収率 99.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

A solution of methyl 2-methoxy-6-methylnicotinate (5.60 g, 30.9 mmol) in dry tetrahydrofuran (155 mL, 30.9 mmol) under an atmosphere of nitrogen was cooled in an ice bath. Lithium aluminum hydride (1.23 g, 30.9 mmol) was added as a slurry in tetrahydrofuran and the mixture was stirred with cooling in an ice bath for 75 minutes. The reaction mixture was diluted with tetrahydrofuran (30 mL). Some Celite® was added followed by sodium sulfate decahydrate to quench. The mixture was filtered and concentrated under vacuum to give (2-methoxy-6-methylpyridin-3-yl)methanol (4.7 g) which was used without purification.

後処理

  1. temperaturewith cooling in an ice bath for 75 minutes
  2. additionSome Celite® was added
  3. customto quench
  4. filtrationThe mixture was filtered
  5. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-8705ef42abdc4b419469809d7be231d6
出典データセット
uspto-grants-2014_09
特許番号
US08841455B2

反応ノート

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