Silane → (3-Mercaptopropyl)trimethoxysilane

HRID 1030840Notes

Reaction equation

HRID 1030840 reaction equation
[SH2:1].[Na].Cl[CH2:4][CH2:5][CH2:6][Si:7]([O:12][CH3:13])([O:10][CH3:11])[O:8][CH3:9].[SiH4]>CN(C)C=O>[SH:1][CH2:4][CH2:5][CH2:6][Si:7]([O:12][CH3:13])([O:10][CH3:11])[O:8][CH3:9]

Participants

5

Reactant 3

HCID 23953SilaneHCID 624493-(Trimethoxysilyl)propyl chlorideHCID 86586439Sodium hydrogen sulphide

Product 1

HCID 20473(3-Mercaptopropyl)trimethoxysilaneYield 84%

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Conditions

Temperature
110 °C

Procedure

566 g (10.1 mols) of sodium hydrogen sulfide together with 2,400 g of dimethylformamide were introduced into the apparatus described in Example 1. While stirring, 2,000 g (10.1 mols) of 3-chloropropyltrimethoxysilane were added to the contents of the flask over a period of 60 minutes, whereby the temperature of the contents of the flask rose to about 100° C. By application of additional heat the temperature was increased to 110° C. and maintained at this level. Samples of the reaction mixture were taken at intervals of 15 minutes and gas-chromatographically analyzed. After the elapse of 75 minutes of reaction time only traces of the provided silane compound could be detected in the reaction mixture. The distillative work-up of the raw reaction mixture gave a yield of 84% of 3-mercaptopropyltrimethoxysilane.

Workup

  1. customrose to about 100° C
  2. temperatureBy application of additional heat the temperature
  3. temperaturemaintained at this level
  4. customwere taken at intervals of 15 minutes and gas-chromatographically
  5. customAfter the elapse of 75 minutes of reaction time
  6. customThe distillative work-up of the raw reaction mixture

Sources & evidence

ORD record
ord-a9a7abe2771e42a09d2ffb16ff8ad9e2
Source dataset
uspto-grants-1992_04
Patent number
US05107009

Reaction notes

Loading…