反応式
[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]参加物
4
反応条件
- 温度
- 80 °C
実験手順
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).
後処理
- customUpon reaching 80° C.
- customthe reaction exothermed to 104° C
- temperatureThe yellow solution was cooled back to 80° C.
- temperatureThe reaction mixture was cooled
出典と根拠
- ORDレコード
- ord-48b6901412864ccaa3a78bc1e1853cf1
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08658568B2
関連ノート
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