Methanol → 5-(4-(2-(trimethoxysilyl)ethyl)benzylthio)-1H-1,2,3-triazole

HRID 2103955노트

반응식

HRID 2103955 반응식
[SH:1][C:2]1[NH:6][N:5]=[N:4][CH:3]=1.ClC[CH:9]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH2:10][Si:11]([O:16][CH3:17])([O:14][CH3:15])[O:12][CH3:13].[CH3:24]O>>[CH3:17][O:16][Si:11]([O:12][CH3:13])([O:14][CH3:15])[CH2:10][CH2:9][C:18]1[CH:19]=[CH:20][C:21]([CH2:24][S:1][C:2]2[NH:6][N:5]=[N:4][CH:3]=2)=[CH:22][CH:23]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 53426825((Chloromethyl)phenylethyl)-trimethoxysilaneHCID 178527741HCID 178527741, 화합물

생성물 1

HCID 1785030005-(4-(2-(trimethoxysilyl)ethyl)benzylthio)-1H-1,2,3-triazole수율 64.8%

실험 절차

10 mmole of 5-mercapto-1H-1,2,3-triazole (sodium salt) was dissolved in 20 ml methanol and stirred for 5 minutes. 10 mmole of ((chloromethyl)phenylethyl)-trimethoxysilane was added to the solution, and stirred for 6 hours. The white precipitate was removed by filtration, the solvent in the filtrate was removed in vacuum. The filtrate was dissolved in small amount of methanol, and separated with a Si gel column (solvents: 5 ethylacetate/5 hexane in volume). 2.2 g product as liquid was obtained. Yield: 64.8%. 1H NMR (CDCl3) of Precursors 5: δ(ppm) 7.47 (1H, s), 7.12 (4H, m), 4.06 (2H, s), 3.55 (9H, s), 2.69 (2H, t, JH-H=8.50), 1.00 (2H, t, JH-H=8.50).

후처리

  1. stirringstirred for 6 hours
  2. customThe white precipitate was removed by filtration
  3. customthe solvent in the filtrate was removed in vacuum
  4. dissolutionThe filtrate was dissolved in small amount of methanol
  5. customseparated with a Si gel column (solvents: 5 ethylacetate/5 hexane in volume)

출처 및 근거

ORD 기록
ord-dad333a9167343bd914c0280500a7950
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576165B2

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