Thionyl Chloride → 2-(Chloromethyl)-6-methylpyridine

HRID 77820

反応式

HRID 77820 の反応式
[CH3:1][C:2]1[N:7]=[C:6]([CH2:8]O)[CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:12])=O>C(Cl)Cl>[Cl:12][CH2:8][C:6]1[CH:5]=[CH:4][CH:3]=[C:2]([CH3:1])[N:7]=1

参加物

4

実験手順

A solution of (6-methyl-pyridin-2-yl)-methanol (1.44 g, 11.7 mmol), thionyl chloride (1.45 mL, 19.9 mmol) and methylene chloride (20 mL) was stirred under reflux for 40 minutes. The reaction solution was cooled to room temperature and then concentrated under a reduced pressure. The residue was partitioned into sodium bicarbonate solution and diethyl ether. The organic layer was concentrated under a reduced pressure, and the residue was purified by silica gel chromatography (ethyl acetate) to obtain the title compound (1.42 g, 85.8%).

後処理

  1. temperatureunder reflux for 40 minutes
  2. concentrationconcentrated under a reduced pressure
  3. customThe residue was partitioned into sodium bicarbonate solution and diethyl ether
  4. concentrationThe organic layer was concentrated under a reduced pressure
  5. customthe residue was purified by silica gel chromatography (ethyl acetate)

出典と根拠

ORDレコード
ord-78e6bd01107849bd8231580d44d84968
出典データセット
uspto-grants-2014_09
特許番号
US08841327B2

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