反応式
[Cl-].[Cl-].[Cl-].[In+3].Cl[SiH](C1C=CC=CC=1)C1C=CC=CC=1.[CH2:19]([N:26]1[CH2:33][CH:32]2[CH:28]([CH:29](O)[C:30]3[CH:36]=[CH:35][S:34][C:31]=32)[CH2:27]1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>ClC(Cl)C>[CH2:19]([N:26]1[CH2:33][CH:32]2[CH:28]([CH2:29][C:30]3[CH:36]=[CH:35][S:34][C:31]=32)[CH2:27]1)[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1参加物
5
反応条件
- 温度
- 60 °C
実験手順
Indiumtrichloride (973 mg, 4.40 mmol) and chlorodiphenylsilane (2888 mg, 13.20 mmol) were added to a solution of the product from step f) (1192 mg, 4.40 mmol) in 20 mL of dichloroethane. The reaction mixture was heated at 60° C. overnight and then was cooled to room temperature and quenched with saturated NaHCO3 (50 ml). The reaction mixture was extracted with ethylacetate (2×50 mL). The combined organic extracts were washed with brine (50 ml), dried with MgSO4 and solvent evaporated in vacuo to afford the subtitle compound (638 mg, yield: 57%) that was used without further purification. MS calculated C16H17NS+H: 256, observed: 256.
後処理
- temperaturewas cooled to room temperature
- customquenched with saturated NaHCO3 (50 ml)
- extractionThe reaction mixture was extracted with ethylacetate (2×50 mL)
- washThe combined organic extracts were washed with brine (50 ml)
- dry with materialdried with MgSO4 and solvent
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-e1aa197d0bd24dc7b74e830b3a5cd79a
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07423056B2
関連ノート
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