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Sodium Hydroxide → HCID 15166268, 화합물

HRID 609845
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HRID 609845 반응식
[OH-].[Na+].[Cl:3][CH2:4][CH2:5][O:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][N:13]=[C:12]([CH2:16]Cl)[C:11]=1[CH3:18].ClCC1C(C)=C(OCCOCCO)C=CN=1.OCC1C(C)=C(OCCOCCO)C=CN=1.[SH:51][C:52]1[NH:56][C:55]2[CH:57]=[CH:58][CH:59]=[CH:60][C:54]=2[N:53]=1>>[Cl:3][CH2:4][CH2:5][O:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][N:13]=[C:12]([CH2:16][S:51][C:52]2[NH:56][C:55]3[CH:57]=[CH:58][CH:59]=[CH:60][C:54]=3[N:53]=2)[C:11]=1[CH3:18]
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참가 물질

6

반응물 5

HCID 14798Sodium HydroxideHCID 19600529HCID 19600529, 화합물HCID 196005412-Hydroxymethyl-4-[2-(2-hydroxyethoxy)ethoxy]-3-methylpyridineHCID 19600542HCID 19600542, 화합물HCID 178527775HCID 178527775, 화합물

생성물 1

HCID 15166268HCID 15166268, 화합물

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온도
60 °C

실험 절차

0.54 g of sodium hydroxide was added to an ethanolic solution of 3.1 g of a crude mixture comprising 4-[2-(2-chloroethoxy)ethoxy]-2-chloromethyl-3-methylpyridine and 2-chloromethyl-4-[2-(2-hydroxy-ethoxy)ethoxy)-3-methylpyridine which has been prepared by the chlorination of 2-hydroxymethyl-4-[2-(2-hydroxyethoxy)ethoxy]-3-methylpyridine and 2.0 g of 2-mercapto-1H-benzimidazole to obtain a mixture. This mixture was stirred at 60° C. for 1.5 hour, cooled and distilled under a reduced pressure to remove the ethanol. The obtained residue was chromatographed over a silica gel column and eluted with ethyl acetate/n-hexane and then with methanol/ethyl acetate to obtain 1.0 g of 2-[{4-(2-(2-chloroethoxy)ethoxy)-3-methylpyridine-2-yl}methylthio]-1H-benzimidazole

후처리

  1. customto obtain a mixture
  2. temperaturecooled
  3. distillationdistilled under a reduced pressure
  4. customto remove the ethanol
  5. customThe obtained residue was chromatographed over a silica gel column
  6. washeluted with ethyl acetate/n-hexane

출처 및 근거

ORD 기록
ord-1f61fb57f01a477588787c5aba446131
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05998445

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