Hydrochloric Acid → 1,3-Divinyltetramethyldisiloxane

HRID 26173

反応式

HRID 26173 の反応式
[CH3:1]Cl.[Mg].Cl[Si:5]([CH:13]=C)([CH3:12])[O:6][Si:7](Cl)([CH:9]=[CH2:10])[CH3:8].[CH3:15][Mg:16][Cl:17].Cl.O1[CH2:23][CH2:22]CC1>O>[CH3:15][Mg:16][Cl:17].[CH:9]([Si:7]([CH3:1])([CH3:8])[O:6][Si:5]([CH:22]=[CH2:23])([CH3:13])[CH3:12])=[CH2:10]

参加物

9

反応物 6

HCID 313Hydrochloric AcidHCID 6327Methyl ChlorideHCID 8028TetrahydrofuranHCID 852011,3-Dichloro-1,3-dimethyl-1,3-divinyldisiloxaneHCID 5462224Magnesium2 回HCID 178418332HCID 178418332、化合物

生成物 2

HCID 758191,3-DivinyltetramethyldisiloxaneHCID 178418332HCID 178418332、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A methyl magnesium chloride solution is prepared by adding methylchloride to a mixture consisting of 1000 milliliters of tetrahydrofuran and 97.2 grams (4 mol) of magnesium in the form of magnesium shavings until the shavings have dissolved. About 400 grams (1.76 mol) of 1,3-dichloro-1,3-divinyl-1,3-dimethyldisiloxane is added dropwise to the methyl magnesium chloride solution with constant agitation and at a temperature between 25° and 75° C. About 1000 milliliters of paraffin oil having a boiling point of about 190° C. at 760 mm Hg (abs), is added, then about 700 milliliters of anhydrous tetrahydrofuran is distilled off until a bath temperature of 150° C. is obtained. The residue obtained from this distillation is mixed with 70 milliliters of water. About 280 milliliters of tetrahydrofuran having a water content of less than 0.5 percent by weight is recovered. After cooling, the residue obtained from the second distillation is mixed with 600 milliliters of water and 100 milliliters of 20 percent aqueous hydrochloric acid and from the organic phase is obtained 317 grams i.e. 94 percent of theoretical, of 1,3-divinyl-1,1,3,3-tetramethyldisiloxane having a boiling point of from 138° to 139° C. and a purity in excess of 98 percent by weight.

後処理

  1. dissolutionhave dissolved
  2. additionis added
  3. distillationabout 700 milliliters of anhydrous tetrahydrofuran is distilled off until a bath temperature of 150° C.
  4. customis obtained
  5. customThe residue obtained from this distillation
  6. customAbout 280 milliliters of tetrahydrofuran having a water content of less than 0.5 percent by weight is recovered
  7. temperatureAfter cooling
  8. customthe residue obtained from the second distillation

出典と根拠

ORDレコード
ord-32012f1931bc44a086a1ce2b2a5e7b15
出典データセット
uspto-grants-1979_04
特許番号
US04148818

関連ノート

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