Water → 2-Chloro-4-(chloromethyl)pyridine

HRID 546567

反応式

HRID 546567 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([CH2:8]O)[CH:5]=[CH:4][N:3]=1.S(Cl)([Cl:12])=O.CN(C)C=O.O>ClCCl>[Cl:1][C:2]1[CH:7]=[C:6]([CH2:8][Cl:12])[CH:5]=[CH:4][N:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 7062237(2-Chloropyridin-4-yl)methanol

生成物 1

HCID 111265732-Chloro-4-(chloromethyl)pyridine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 11.3 g of 2-chloro-4-hydroxymethylpyridine obtained in stage a) below in 200 mL of dichloromethane are added dropwise 6.896 mL of thionyl chloride, followed by 2.1 mL of dimethylformamide, the reaction mixture is stirred for 3 hours at room temperature and 50 mL of water are then added dropwise. The phases are separated and the organic phase is washed with water, dried over magnesium sulphate, filtered and concentrated under reduced pressure to give 12.8 g of 2-chloro-4-chloromethylpyridine in the form of an amber-coloured liquid, which is used without further purification.

後処理

  1. customThe phases are separated
  2. washthe organic phase is washed with water
  3. dry with materialdried over magnesium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-92422a956bf04cd28d557a55a375e905
出典データセット
uspto-grants-2011_05
特許番号
US07935819B2

関連ノート

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