Tributylstannane → (E)-1-tri-n-butylstannyl-3-triethylsilyloxy-1-octene

HRID 1632692노트

반응식

HRID 1632692 반응식
[CH2:1]([Si:3]([CH2:15][CH3:16])([CH2:13][CH3:14])[O:4][CH:5]([CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[C:6]#[CH:7])[CH3:2].N(C(C)(C)C#N)=NC(C)(C)C#N.[CH2:29]([SnH:33]([CH2:38][CH2:39][CH2:40][CH3:41])[CH2:34][CH2:35][CH2:36][CH3:37])[CH2:30][CH2:31][CH3:32]>>[CH2:38]([Sn:33]([CH2:29][CH2:30][CH2:31][CH3:32])([CH2:34][CH2:35][CH2:36][CH3:37])/[CH:7]=[CH:6]/[CH:5]([O:4][Si:3]([CH2:13][CH3:14])([CH2:1][CH3:2])[CH2:15][CH3:16])[CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[CH2:39][CH2:40][CH3:41]

참가 물질

4

반응물 3

HCID 5948TributylstannaneHCID 6547AzobisisobutyronitrileHCID 126753463-Triethylsilyloxy-1-octyne

생성물 1

HCID 20442056(E)-1-tri-n-butylstannyl-3-triethylsilyloxy-1-octene

실험 절차

A solution of 20 g of 3-triethylsilyloxy-1-octyne, 150 mg of azobisisobutyronitrile, and 30 ml of tri-n-butyltin hydride is magnetically stirred un er an argon atmosphere at 140° C. for 2 hours, (EXOTHERMIC), then cooled to ambient temperature. The excess tin hydride is removed by distillation (~70°/1.0 mm). The residue is purified by distillation to provide 36.5 g of the oil (bp 165° C. at 0.05 mm).

후처리

  1. customat 140° C.
  2. customfor 2 hours
  3. customThe excess tin hydride is removed by distillation (~70°/1.0 mm)
  4. distillationThe residue is purified by distillation

출처 및 근거

ORD 기록
ord-dfe125626b584e11bb602936496cbed6
출처 데이터셋
uspto-grants-1984_10
특허 번호
US04477388

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