Tetrahydrofuran → Chloropropyldimethylvinylsilane

HRID 1170068

반응식

HRID 1170068 반응식
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]

참가 물질

4

반응물 3

HCID 8028TetrahydrofuranHCID 82765Silane, chloro(3-chloropropyl)dimethyl-HCID 178418507HCID 178418507, 화합물

생성물 1

HCID 131715857Chloropropyldimethylvinylsilane수율 66.49%

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-b4d53911fb1348868ab25b31f34d2f40
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07825257B1

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