1,2-Bis(2-iodoethoxy)ethane → 1,2-bis(2-(3H-1,2,3-triazol-4-ylthio)ethoxy)ethane

HRID 2103944노트

반응식

HRID 2103944 반응식
I[CH2:2][CH2:3][O:4][CH2:5][CH2:6][O:7][CH2:8][CH2:9]I.[SH:11][C:12]1[NH:16][N:15]=[N:14][CH:13]=1>C(O)C>[N:14]1[CH:13]=[C:12]([S:11][CH2:2][CH2:3][O:4][CH2:5][CH2:6][O:7][CH2:8][CH2:9][S:11][C:12]2[NH:16][N:15]=[N:14][CH:13]=2)[NH:16][N:15]=1

참가 물질

4

반응물 2

HCID 5934361,2-Bis(2-iodoethoxy)ethaneHCID 178527741HCID 178527741, 화합물

생성물 1

HCID 1784209301,2-bis(2-(3H-1,2,3-triazol-4-ylthio)ethoxy)ethane수율 88%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

10 ml of 1,2-bis(2-iodoethoxy)-ethane was dropped into the solution of 20 mmole 5-mercapto-1H-1,2,3-triazole (sodium salt) in 20 ml ethanol, and stirred for 24 hours at room temperature. After the solvent was evaporated in vacuum, the residual was separated with silica gel column. Elution with hexane/ethylacetate (1/3) first, and then with pure ethyl acetate gave 2.70 g product as viscous solid. Yield: 88%. 1H NMR (CDCl3): δ(ppm) 7.72 (2H, s), 3.74 (4H, t, JH-H=6.19), 3.65 (4H, s), 3.07 (4H, t, JH-H=6.19).

후처리

  1. customAfter the solvent was evaporated in vacuum
  2. customthe residual was separated with silica gel column
  3. washElution with hexane/ethylacetate (1/3) first

출처 및 근거

ORD 기록
ord-daa5aa3cc4414293803f006ab10e6f03
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576165B2

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