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

HRID 2103944ノート

反応式

HRID 2103944 の反応式
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

参加物

4

反応物 2

HCID 5934361,2-Bis(2-iodoethoxy)ethaneHCID 178527741HCID 178527741、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-daa5aa3cc4414293803f006ab10e6f03
出典データセット
uspto-grants-2009_08
特許番号
US07576165B2

反応ノート

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