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Methyl iodide → 3-(Methoxymethyl)pyridine

HRID 1913744
ノート
印刷プレビュー

反応式

HRID 1913744 の反応式
[OH:1][CH2:2][C:3]1[CH:4]=[N:5][CH:6]=[CH:7][CH:8]=1.[CH2:9]1COCC1.[H-].[Na+].CI>O>[CH3:9][O:1][CH2:2][C:3]1[CH:4]=[N:5][CH:6]=[CH:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 75103-PyridinemethanolHCID 8028TetrahydrofuranHCID 24758Sodium hydride

生成物 1

HCID 3389263-(Methoxymethyl)pyridine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a mixture of 10.0 g of 3-hydroxymethylpyridine and 200 ml of THF, 3.7 g of 60% sodium hydride (in oil) was added in small portions at room temperature and then stirred for 15 minutes. To the reaction mixture, 13.0 g of methyl iodide was added dropwise, and the reaction mixture was stirred at room temperature for three hours. To the reaction mixture, 25 ml of water was added. Then, the reaction mixture was concentrated under reduced pressure. To the residue, 25 ml of water was added, followed by extraction with ethyl acetate three times. The combined organic layers were washed with a saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 8.17 g of 3-methoxymethylpyridine.

後処理

  1. additionwas added in small portions at room temperature
  2. stirringthe reaction mixture was stirred at room temperature for three hours
  3. concentrationThen, the reaction mixture was concentrated under reduced pressure
  4. additionTo the residue, 25 ml of water was added
  5. extractionfollowed by extraction with ethyl acetate three times
  6. washThe combined organic layers were washed with a saturated sodium chloride solution
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-66e83ca908394659a6fb5ca7d53036fb
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08609705B2

反応ノート

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