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Water → 3-(Methoxymethyl)pyridine

HRID 1005375
ノート
印刷プレビュー

反応式

HRID 1005375 の反応式
[OH:1][CH2:2][C:3]1[CH:4]=[N:5][CH:6]=[CH:7][CH:8]=1.[H-].[Na+].I[CH3:12].O>O1CCCC1>[CH3:12][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 962WaterHCID 6328Methyl iodideHCID 75103-PyridinemethanolHCID 24758Sodium hydride

生成物 1

HCID 3389263-(Methoxymethyl)pyridine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 3-hydroxymethylpyridine (10 g, 92 mmol) in anhydrous tetrahydrofuran (200 ml), under an atmosphere of nitrogen, was treated with sodium hydride (4 g of a 55% oil dispersion, 92 mmol) in portions. After stirring for 15 minutes iodomethane (5.7 ml, 92 mmol) was added dropwise and the reaction mixture was stirred at ambient temperature for 2 hours. Water (20 ml) was added and the tetrahydrofuran evaporated. The residue was partitioned between water (50 ml) and dichloromethane (70 ml). The organic layer was separated, dried (sodium sulphate) then evaporated. The crude product was purified by column chromatography on silica using ethyl acetate. The title compound was obtained (11 g, 93%) as an oil, δH (250 MHz, CDCl3) 3.42 (3H, s), 4.48 (2H, s), 7.27-7.32 (1H, m), 7.66-7.71 (1H, m), 8.53-8.60 (2H, m).

後処理

  1. additionwas added dropwise
  2. customthe tetrahydrofuran evaporated
  3. customThe residue was partitioned between water (50 ml) and dichloromethane (70 ml)
  4. customThe organic layer was separated
  5. dry with materialdried (sodium sulphate)
  6. customthen evaporated
  7. customThe crude product was purified by column chromatography on silica

出典と根拠

ORDレコード
ord-851e06dd801c4fc3807b95b8707281b1
出典データセット
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06054469

反応ノート

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