2-Methylpyridine → 2-Methyl-1-[2-oxo-2-(tetrahydro-pyran-4-yl)-ethyl]-pyridinium bromide

HRID 37824

反応式

HRID 37824 の反応式
[Br:1][CH2:2][C:3]([CH:5]1[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1)=[O:4].[N:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[CH3:17]>CO>[Br-:1].[CH3:17][C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][N+:11]=1[CH2:2][C:3](=[O:4])[CH:5]1[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1

参加物

4

反応物 2

HCID 79752-MethylpyridineHCID 131972252-Bromo-1-(oxan-4-yl)ethan-1-one

生成物 1

HCID 866496902-Methyl-1-[2-oxo-2-(tetrahydro-pyran-4-yl)-ethyl]-pyridinium bromide収率 86.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 2-bromo-1-(tetrahydro-pyran-4-yl)-ethanone (0.6 g, 2.89 mmol) and 2-picoline (0.4 mL, 4.3 mmol) in methanol (10 mL) was heated to reflux and maintained overnight. The solvent was removed in vacuo to give a residue which was washed with 20% ethyl acetate in hexane to afford 2-methyl-1-[2-oxo-2-(tetrahydro-pyran-4-yl)-ethyl]-pyridinium bromide (0.75 g, 86%) as a semi-solid.

後処理

  1. temperaturewas heated
  2. temperatureto reflux
  3. temperaturemaintained overnight
  4. customThe solvent was removed in vacuo
  5. customto give a residue which
  6. washwas washed with 20% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-203bea987b4746448a898a969cf61fa0
出典データセット
uspto-grants-2013_09
特許番号
US08524705B2

関連ノート

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