Dichloromethane → HCID 178503002, compound

HRID 1808671Notes

Reaction equation

HRID 1808671 reaction equation
[NH:1]1[CH:5]=[N:4][CH:3]=[N:2]1.[H-].[Na+].I[CH2:9][CH2:10][CH2:11][Si:12]([O:17][CH3:18])([O:15][CH3:16])[O:13][CH3:14].ClCCl>O1CCCC1>[CH3:14][O:13][Si:12]([CH2:11][CH2:10][CH2:9][C:5]1[N:4]=[CH:3][NH:2][N:1]=1)([O:17][CH3:18])[O:15][CH3:16]

Participants

6

Reactant 4

HCID 6344DichloromethaneHCID 92571H-1,2,4-TriazoleHCID 24758Sodium hydrideHCID 2759373(3-Iodopropyl)trimethoxysilane

Product 1

HCID 178503002HCID 178503002, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

5 g (72 mmol) of 1,2,4-triazole were dissolved in 100 ml of absolute tetrahydrofurane and 1.73 g (72 mmol) of sodium hydride were added. The reaction mixture was stirred for 4 hours, after which 10 ml of iodopropyltrimethoxy silane (52 mmol) were added and the reaction mixture was heated under reflux for 18 hours. 20 ml of dichloromethane were then added and the reaction mixture was filtered. The solvent was removed at 150-155° C. under reduced pressure (8 mbar) and then filtered. The yield was 6.4 g (50%).

Workup

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 18 hours
  3. filtrationthe reaction mixture was filtered
  4. customThe solvent was removed at 150-155° C. under reduced pressure (8 mbar)
  5. filtrationfiltered

Sources & evidence

ORD record
ord-b9122c1815fe44b389e2c94b1dfb185b
Source dataset
uspto-grants-2013_01
Patent number
US08361627B2

Reaction notes

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