関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 反応物 | 7-Amino-4-(4-hydroxy-3-methoxyphenyl)isoindolinone | HCID 68487661 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 68490965 | HCID 68490965 | 72% |
反応手順
7-Amino-4-(4-hydroxy-3-methoxyphenyl)isoindolinone (50.0 mg, 0.185 mmol) was dissolved in acetonitrile (2.5 mL), and the solution was added with tert-butyldimethylsilyl chloride (33.5 mg, 0.222 mmol), 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) (0.033 mL, 0.22 mmol), followed by stirring at room temperature for 1.3 hours. The mixture was added with tert-butyldimethylsilyl chloride (33.5 mg, 0.222 mmol) and DBU (0.033 mL, 0.22 mmol), followed by further stirring for 1 hour. The reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by preparative thin-layer chromatography (chloroform/acetonitrile=2/1) to obtain 7-amino-4-(4-tert-butyldimethylsilyloxy-3-methoxyphenyl)isoindolinone (51.1 mg, yield 72%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07745641B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-78c5d8d1945d4cd0a61a9be59df50545 |
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| 出典メモ | uspto-grants-2010_06 |
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