反応式
Cl[CH2:2][Si:3]([CH3:6])([CH3:5])[CH3:4].[CH2:7]([NH2:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(=O)([O-])[O-].[K+].[K+]>>[CH2:7]([NH:14][CH2:2][Si:3]([CH3:6])([CH3:5])[CH3:4])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1参加物
4
反応条件
- 温度
- 120 °C
実験手順
A mixture of chloromethyltrimethylsilane (325g, 370 ml, 2.65 mole) and benzylamine (835 g, 850 ml, 7.78 mole) was heated at 120° C. (oil bath temperature) for 2 h. A white solid began appearing after only 10 minutes and a viscous mixture eventually resulted. The reaction mixture was allowed to cool, then basified with potassium carbonate solution and extracted twice with ether. The combined extracts were dried (Na2SO4) and concentrated in vacuo to leave a yellow oil, which was purified by distillation. The excess benzylamine was removed in the first fractions (b.p. 47°-62° C. at 2 mmHg). The title compound (D10) was obtained as a colourless oil (380 g, 74%) b.p. 75°-80° C. at 2 mmHg.
後処理
- customa viscous mixture eventually resulted
- temperatureto cool
- extractionextracted twice with ether
- dry with materialThe combined extracts were dried (Na2SO4)
- concentrationconcentrated in vacuo
- customto leave a yellow oil, which
- distillationwas purified by distillation
- customThe excess benzylamine was removed in the first fractions (b.p. 47°-62° C. at 2 mmHg)
出典と根拠
- ORDレコード
- ord-c3e2d58493ae4b80a2f18d2a5f6e8769
- 出典データセット
- uspto-grants-1992_11
- 特許番号
- US05166357
関連ノート
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