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Water → 2,6-dichloro-4-(chloromethyl)pyridine

HRID 651430
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HRID 651430 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([CH2:8]O)[CH:5]=[C:4]([Cl:10])[N:3]=1.N1C=CC=CC=1.S(Cl)([Cl:19])=O.O>C1(C)C=CC=CC=1.C(OCC)C>[Cl:1][C:2]1[CH:7]=[C:6]([CH2:8][Cl:19])[CH:5]=[C:4]([Cl:10])[N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 1049PyridineHCID 24386Thionyl ChlorideHCID 2794840(2,6-Dichloropyridin-4-yl)methanol

생성물 1

HCID 27946262,6-dichloro-4-(chloromethyl)pyridine

시약·촉매·용매 2

HCID 1140Toluene용매HCID 3283
이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트
Diethyl Ether
용매

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온도
110 °C

실험 절차

5.0 g of 2,6-dichloro-4-pyridinemethanol and 2.5 ml of pyridine were suspended in 10 ml of toluene, and the suspension was cooled in a salt-ice bath. To this, 2.7 ml of thionyl chloride were added dropwise for 1 hour, and subsequently the reacted solution was stirred at 110° C. for 3 hours. After cooling, water was added to the solution, and extraction was conducted using diethyl ether. The organic phase was washed with water, and was dried by adding sodium sulfate. The solvent was removed by evaporation, and the residue was purified by silica gel column chromatography to obtain 5.0 g of 2,6-dichloro-4-chloromethylpyridine.

후처리

  1. temperaturethe suspension was cooled in a salt-ice bath
  2. temperatureAfter cooling
  3. washThe organic phase was washed with water
  4. customwas dried
  5. additionby adding sodium sulfate
  6. customThe solvent was removed by evaporation
  7. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-8c45572ba7e041ae867c31cb16f18797
출처 데이터셋
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06281231B1

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