Tributylstannane → (E)-triethoxy(2-(tributylstannyl)vinyl)silane

HRID 244305

반응식

HRID 244305 반응식
[CH2:1]([SnH:5]([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].[CH2:14]([O:16][Si:17]([O:23][CH2:24][CH3:25])([O:20][CH2:21][CH3:22])[C:18]#[CH:19])[CH3:15]>CC(N=NC(C#N)(C)C)(C#N)C>[CH2:21]([O:20][Si:17]([O:23][CH2:24][CH3:25])([O:16][CH2:14][CH3:15])/[CH:18]=[CH:19]/[Sn:5]([CH2:1][CH2:2][CH2:3][CH3:4])([CH2:6][CH2:7][CH2:8][CH3:9])[CH2:10][CH2:11][CH2:12][CH3:13])[CH3:22]

참가 물질

4

반응물 2

HCID 5948TributylstannaneHCID 79778Silane, triethoxyethynyl-

생성물 1

HCID 86668310(E)-triethoxy(2-(tributylstannyl)vinyl)silane수율 101.4%

시약·촉매·용매 1

HCID 6547Azobisisobutyronitrile촉매

반응 조건

온도
80 °C

실험 절차

Tributyltin hydride (1.9 mL, 7.2 mmol, 1.0 equiv) and triethoxy(ethynyl)silane (1.5 g, 7.9 mmol, 1.1 equiv) were combined. AIBN (60 mg, 0.36 mmol, 0.05 equiv) was added and the resulting yellow solution was heated to 80° C. Upon reaching 80° C., the reaction exothermed to 104° C. The yellow solution was cooled back to 80° C. and stirred for 20 h. The reaction mixture was cooled to provide the title compound as a pale yellow oil (3.5 g, 99% crude yield): IR (thin film) 2957 (s), 2925 (s), 2873 (m), 2854 (m) cm−1; 1H NMR (400 MHz, CDCl3) δ 7.43 (d, J=24 Hz, 1H), 6.37 (d, J=24 Hz, 1H), 3.83 (q, J=7 Hz, 6H), 1.49 (m, 6H), 1.29 (m, 6H), 1.22 (t, J=7 Hz, 9 H), 0.82-0.92 (m, 15 H).

후처리

  1. customUpon reaching 80° C.
  2. customthe reaction exothermed to 104° C
  3. temperatureThe yellow solution was cooled back to 80° C.
  4. temperatureThe reaction mixture was cooled

출처 및 근거

ORD 기록
ord-48b6901412864ccaa3a78bc1e1853cf1
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658568B2

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