Tetrahydrofuran → Chloropropyldimethylvinylsilane

HRID 1170068

反応式

HRID 1170068 の反応式
C([Mg]Br)=C.[Cl:5][CH2:6][CH2:7][CH2:8][Si:9]([CH3:12])(C)Cl.[CH2:13]1[CH2:17]OC[CH2:14]1>>[Cl:5][CH2:6][CH2:7][CH2:8][SiH2:9][CH:12]=[C:13]([CH3:17])[CH3:14]

参加物

4

反応物 3

HCID 8028TetrahydrofuranHCID 82765Silane, chloro(3-chloropropyl)dimethyl-HCID 178418507HCID 178418507、化合物

生成物 1

HCID 131715857Chloropropyldimethylvinylsilane収率 66.49%

実験手順

To a stirred solution of 1 M vinyl magnesium bromide in THF (9.1 L), 3-chloropropyl dimethylchlorosilane (1.5 Kg) was added over the period of 3 hr through an addition. The reaction mixture stirred further for 2 hr. Added D.M water (9.1 L) and separated the organic layer. The hazy aqueous layer was filtered through hyflo bed and extracted with dichloromethane (3.0 L). The dichloromethane extract was mixed with organic layer and evaporated to dryness to give yellow liquid which was distilled using a Vigreaux column to get pure colorless title product (0.986 Kg)

後処理

  1. customAdded D.M water (9.1 L) and separated the organic layer
  2. filtrationThe hazy aqueous layer was filtered through hyflo bed
  3. extractionextracted with dichloromethane (3.0 L)
  4. extractionThe dichloromethane extract
  5. additionwas mixed with organic layer
  6. customevaporated to dryness
  7. customto give yellow liquid which
  8. distillationwas distilled

出典と根拠

ORDレコード
ord-b4d53911fb1348868ab25b31f34d2f40
出典データセット
uspto-grants-2010_11
特許番号
US07825257B1

関連ノート

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