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Thionyl Chloride → 2-Chloro-4-(chloromethyl)-6-methoxypyridine hydrochloride

HRID 1384617
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HRID 1384617 반응식
S(Cl)([Cl:3])=O.[Cl:5][C:6]1[CH:11]=[C:10]([CH2:12]O)[CH:9]=[C:8]([O:14][CH3:15])[N:7]=1>C1(C)C=CC=CC=1>[ClH:3].[Cl:5][C:6]1[CH:11]=[C:10]([CH2:12][Cl:3])[CH:9]=[C:8]([O:14][CH3:15])[N:7]=1
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참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 11457961(2-Chloro-6-methoxypyridin-4-yl)methanol

생성물 1

HCID 226250592-Chloro-4-(chloromethyl)-6-methoxypyridine hydrochloride수율 74%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Thionyl chloride (1.0 ml) was added to a solution of 2-chloro-4-hydroxymethyl-6-methoxypyridine (0.9 g, 5.2 mmol) in toluene 10 ml) and the mixture stirred at ambient temperature for 1 hour. The volatiles were removed by evaporation, the residue was azeotroped with toluene and dried under vacuum to give 2-chloro-4-chloromethyl-6-methoxypyridine hydrochloride (0.88 g, 74%). 1H NMR Spectrum: (DMSOd6) 3.85(s, 3H); 4.70(s, 2H); 6.90(s, 1H); 7.15(s, 1H)

후처리

  1. customThe volatiles were removed by evaporation
  2. customthe residue was azeotroped with toluene
  3. customdried under vacuum

출처 및 근거

ORD 기록
ord-f61b79e1cae54c609715831329eb3332
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06258951B1

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