Reaction equation
[O-:1][CH2:2][CH3:3].[Na+].[S:5]1[CH:9]=[CH:8][CH:7]=C1CC(O)=O.ClCCC[Si:18]([O:25][CH2:26][CH3:27])([O:22][CH2:23][CH3:24])[O:19][CH2:20][CH3:21]>S1C=CC=C1C(O)=O.C(O)C>[C:2]([S:5][CH2:9][CH2:8][CH2:7][Si:18]([O:25][CH2:26][CH3:27])([O:22][CH2:23][CH3:24])[O:19][CH2:20][CH3:21])(=[O:1])[CH3:3]Participants
Procedure
This example illustrates the preparation of a thiocarboxylate alkoxysilane from a salt of a thiolcarboxylic acid using as a solvent the alcohol corresponding to the silane alkoxy group. Into a 250 ml, three-neck round bottomed flask equipped with magnetic stir bar, temperature probe/controller, heating mantle, addition funnel, condenser, and N2 inlet was charged 63 grams of a 21 weight percent sodium ethoxide in ethanol. Fifteen grams of thiolacetic acid was added slowly, keeping the temperature below 65° C. The solution was allowed to cool to room temperature, and 48 grams of chloropropyltriethoxysilane was added via the addition funnel. After addition was complete, the solution was heated to 70° C. for 24 hours whereupon a white solid formed. Analysis of the solution by gas chromatography showed a 78 percent yield of acetylthiopropyltriethoxysilane.
Workup
- customInto a 250 ml, three-neck round bottomed flask equipped with magnetic stir bar
- temperaturetemperature probe/controller, heating mantle
- additionaddition funnel, condenser, and N2 inlet
- customthe temperature below 65° C
- additionAfter addition
- temperaturethe solution was heated to 70° C. for 24 hours whereupon a white solid
- customformed
Sources & evidence
- ORD record
- ord-3910189f7bc84d7493667a0e713c210c
- Source dataset
- uspto-grants-2006_10
- Patent number
- US07122590B2
Linked notes
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