Thionyl Chloride → 2-Chloro-5-chloromethylpyridine hydrochloride

HRID 249484

反応式

HRID 249484 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8]O)=[CH:4][CH:3]=1.S(Cl)([Cl:12])=O>C(Cl)(Cl)Cl.CCOCC>[ClH:1].[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][Cl:12])=[CH:4][CH:3]=1

参加物

5

反応物 2

HCID 24386Thionyl ChlorideHCID 177161(6-Chloropyridin-3-yl)methanol

生成物 1

HCID 224503272-Chloro-5-chloromethylpyridine hydrochloride

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6212Chloroform溶媒

実験手順

In 500 ml of CHCl3 was dissolved 47.3 g (0.33 mole) of 6-chloro-3-pyridylmethanol followed by dropwise addition of 99.3 ml of thionyl chloride with stirring at room temperature. After completion of the dropwise addition, the mixture was further stirred for 1.5 hours and, then, allowed to stand overnight. The CHCl3 was distilled off under reduced pressure, whereby crystals and oil were obtained as a residue. The residue was diluted with ether, collected by filtration and dried to give 45.2 g of 6-chloro-3-pyridylmethyl chloride hydrochloride as white crystals.

後処理

  1. additionAfter completion of the dropwise addition
  2. stirringthe mixture was further stirred for 1.5 hours
  3. distillationThe CHCl3 was distilled off under reduced pressure, whereby crystals
  4. customoil were obtained as a residue
  5. filtrationcollected by filtration
  6. customdried

出典と根拠

ORDレコード
ord-fc73b76b5b754717952b85f0f2a4cd82
出典データセット
uspto-grants-1993_05
特許番号
US05214152

関連ノート

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