Methyltrimethoxysilane → methyltri-methoxysilane 3,3,3-trifluoropropyltrimethoxysilane KOH

HRID 404940

反応式

HRID 404940 の反応式
[CH3:1][Si:2]([O:7][CH3:8])([O:5][CH3:6])[O:3][CH3:4].[F:9][C:10]([F:21])([F:20])[CH2:11][CH2:12][Si:13]([O:18][CH3:19])([O:16][CH3:17])[O:14][CH3:15].[OH-:22].[K+:23]>O>[CH3:1][Si:2]([O:7][CH3:8])([O:5][CH3:6])[O:3][CH3:4].[F:21][C:10]([F:9])([F:20])[CH2:11][CH2:12][Si:13]([O:14][CH3:15])([O:18][CH3:19])[O:16][CH3:17].[OH-:22].[K+:23]

参加物

5

反応物 3

HCID 14456MethyltrimethoxysilaneHCID 14797Potassium Hydroxide2 回HCID 679333,3,3-Trifluoropropyl-trimethoxysilane

生成物 1

HCID 86686442methyltri-methoxysilane 3,3,3-trifluoropropyltrimethoxysilane KOH

試薬・触媒・溶媒 1

HCID 962Water溶媒4 回

反応条件

温度
70 °C

実験手順

A 500 ml 5-neck round-bottom flask, rendered inert with nitrogen and equipped with paddle stirrer, dropping funnel, thermometer, and water separator with reflux condenser, is charged with 50 g (0.36 mol) of methyl-trimethoxysilane (available commercially from Wacker Chemie AG), 8.8 g (0.04 mol) of 3,3,3-trifluoro-propyltrimethoxysilane (available commercially from Fluka), and 39.7 g of Isopar E (isoparaffinic hydro-carbon mixture having a boiling range of 113-143° C., available commercially from ExxonMobil). The water separator is filled to the brim with Isopar E. Accompanied by stirring at 350 rpm, a solution of 17.2 g of potassium hydroxide (85% strength, available commercially from AppliChem) (0.26 mol of potassium hydroxide) and 15.3 g of demineralized water is metered in over 12 minutes. During this metered addition, the mixture heats up to 67° C. The mixture is heated to boiling temperature (70° C.). The distillate separates out as the bottom phase in the water separator. Up to a boiling temperature of 119° C., 48.5 g of colorless, slightly turbid distillate accumulate. The suspension which remains is subsequently evaporated to dryness with stirring under a full oil-pump vacuum (5 hPa) to 70° C. This gives 45.9 g of fine, white, free-flowable powder with a solids content of 99.7% (determined using the HR73 halogen moisture analyzer from Mettler Toledo at 160° C.). A 50% strength aqueous solution prepared with this powder exhibits no precipitation even after being stored at room temperature for two weeks in the absence of air.

後処理

  1. customA 500 ml 5-neck round-bottom flask, rendered inert with nitrogen
  2. customequipped with paddle stirrer
  3. temperaturewith reflux condenser
  4. customis metered in over 12 minutes
  5. additionDuring this metered addition
  6. customheats up to 67° C
  7. customThe suspension which remains is subsequently evaporated to dryness
  8. stirringwith stirring under a full oil-pump vacuum (5 hPa) to 70° C
  9. customat 160° C.
  10. customA 50% strength aqueous solution prepared with this powder
  11. customno precipitation even
  12. waitafter being stored at room temperature for two weeks in the absence of air

出典と根拠

ORDレコード
ord-f03e6d9130f142adb661f6788c4ff961
出典データセット
uspto-grants-2014_06
特許番号
US08748645B2

関連ノート

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