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Thionyl Chloride → 2-Chloromethyl-4-(2-hydroxyethoxy)-3-methylpyridine

HRID 357551
ノート
印刷プレビュー

反応式

HRID 357551 の反応式
[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([CH2:11]O)[C:6]=1[CH3:13].S(Cl)([Cl:16])=O>ClCCl>[Cl:16][CH2:11][C:7]1[C:6]([CH3:13])=[C:5]([O:4][CH2:3][CH2:2][OH:1])[CH:10]=[CH:9][N: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

4

反応物 2

HCID 24386Thionyl ChlorideHCID 196005474-(2-Hydroxyethoxy)-2-hydroxymethyl-3-methylpyridine

生成物 1

HCID 151662222-Chloromethyl-4-(2-hydroxyethoxy)-3-methylpyridine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

11.9 g of the 4-(2-hydroxyethoxy)-2-hydroxymethyl-3-methylpyridine prepared above was dissolved in 200 ml of dichloromethane to obtain a solution. 24 ml of thionyl chloride was dropwise added to this solution at 0° C. The obtained mixture was stirred at a room temperature for 2 hours and distilled under a reduced pressure to remove the dichloromethane and excess thionyl chloride. A saturated aqueous solution of sodium hydrogencarbonate was added to the residue to obtain a mixture. This mixture was extracted with chloroform. The extract was dried over magnesium sulfate and filtered. The filtrate was concentrated to obtain 10.9 g of 2-chloromethyl-4-(2-hydroxyethoxy)-3-methylpyridine.

後処理

  1. customto obtain a solution
  2. distillationdistilled under a reduced pressure
  3. customto remove the dichloromethane and excess thionyl chloride
  4. additionA saturated aqueous solution of sodium hydrogencarbonate was added to the residue
  5. customto obtain a mixture
  6. extractionThis mixture was extracted with chloroform
  7. dry with materialThe extract was dried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-d070cc435bc64dafa95e29cadc52d625
出典データセット
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05840910

反応ノート

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