Thionyl Chloride → 2-Chloro-5-chloromethylpyridine hydrochloride

HRID 249484노트

반응식

HRID 249484 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 224503272-Chloro-5-chloromethylpyridine hydrochloride

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fc73b76b5b754717952b85f0f2a4cd82
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05214152

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