1,8-Diiodooctane → HCID 178420908, compound

HRID 2103943Notes

Reaction equation

HRID 2103943 reaction equation
[SH:1][C:2]1[N:6]=[CH:5][NH:4][N:3]=1.I[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]I>C(O)C>[NH:4]1[CH:5]=[N:6][C:2]([S:1][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][S:1][C:2]2[N:6]=[CH:5][NH:4][N:3]=2)=[N:3]1

Participants

4

Reactant 2

HCID 906051,8-DiiodooctaneHCID 178527894HCID 178527894, compound2×

Product 1

HCID 178420908HCID 178420908, compoundYield 35.2%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

20 mmole of 3-mercapto-1H-1,2,4-triazole (potassium salt) was dissolved in 20 ml of ethanol in stirring. 10 mmole of 1,8-diiodooctane was added dropwise to the solution of 3-mercapto-1H-1,2,4-triazole (potassium salt), and stirred overnight. After the solvent was evaporated in vacuum, the residual was washed with 50 ml pure H2O for three times, and then with 50 ml hexane for 3 times. At last, the residual was dried in oven at 60° C. for 24 hours. 1.1 g product was obtained as white solid. Yield: 30%. 1H NMR (DMSO): δ(ppm) 8.34 (2H, s), 3.04 (4H, t, JH-H=7.14), 1.61 (4H, m), and 1.23-1.32 (8H, m).

Workup

  1. stirringstirred overnight
  2. customAfter the solvent was evaporated in vacuum
  3. washthe residual was washed with 50 ml pure H2O for three times
  4. customAt last, the residual was dried in oven at 60° C. for 24 hours

Sources & evidence

ORD record
ord-f7b6582781a74d669b4c152c14fb3e36
Source dataset
uspto-grants-2009_08
Patent number
US07576165B2

Reaction notes

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