Sodium ethoxide → 3-[Ethoxy(dimethyl)silyl]propane-1-thiol
反応式
C([S:4][CH2:5][CH2:6][CH2:7][Si:8]([O:11][CH2:12][CH3:13])([CH3:10])[CH3:9])(=O)C.CC[O-].[Na+]>C(O)C>[SH:4][CH2:5][CH2:6][CH2:7][Si:8]([O:11][CH2:12][CH3:13])([CH3:10])[CH3:9]参加物
4
実験手順
Added, at ambient temperature, to a solution of S-(ethanoyl)mercaptopropylethoxydimethylsilane C (65.4 g, 0.297 mol) in absolute ethanol (230 ml) is solid sodium ethylate (2.02 g, 0.030 mol) under argon. The reaction medium is brought to reflux for 2.5 hours. After returning to ambient temperature, the precipitate of NaCl is filtered and washed with heptane (350 ml). After evaporating the solvents under reduced pressure at 45° C., the oil obtained is purified by vacuum distillation (60° C./10 mbar). The 3-mercaptopropylethoxydimethylsilane D with CAS number [141137-15-7] (34.7 g, 0.195 mol) is obtained with a yield of 66%.
後処理
- temperatureto reflux for 2.5 hours
- customAfter returning to ambient temperature
- filtrationthe precipitate of NaCl is filtered
- washwashed with heptane (350 ml)
- customAfter evaporating the solvents under reduced pressure at 45° C.
- customthe oil obtained
- distillationis purified by vacuum distillation (60° C./10 mbar)
出典と根拠
- ORDレコード
- ord-f3d24dadaf68443183f854cf8327cb92
- 出典データセット
- uspto-grants-2015_04
- 特許番号
- US09000092B2
反応ノート
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