2-Thiopheneacetic acid → S-[3-(Triethoxysilyl)propyl] ethanethioate

HRID 1793223

反応式

HRID 1793223 の反応式
[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]

参加物

6

反応物 3

HCID 159702-Thiopheneacetic acidHCID 78771(3-Chloropropyl)triethoxysilaneHCID 2723922Sodium ethoxide

生成物 1

HCID 21922028S-[3-(Triethoxysilyl)propyl] ethanethioate収率 78%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 107002-Thiophenecarboxylic acid溶媒

実験手順

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 3-(acetylthio)-1-propyltriethoxysilane.

後処理

  1. customInto a 250 ml, three-neck round bottomed flask equipped with magnetic stir bar
  2. temperaturetemperature probe/controller, heating mantle
  3. additionaddition funnel, condenser, and N2 inlet
  4. customthe temperature below 65° C
  5. additionAfter addition
  6. temperaturethe solution was heated to 70° C. for 24 hours whereupon a white solid
  7. customformed

出典と根拠

ORDレコード
ord-a2cdc9ab8298469c92bf748bc8239564
出典データセット
uspto-grants-2006_07
特許番号
US07078551B2

関連ノート

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