関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phthalimide potassium salt | HCID 24194345 | — |
| 反応物 | 2-(4-Chlorophenyl)-2-(4-iodophenyl)oxirane | HCID 59317217 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-[2-(4-Chloro-phenyl)-2-hydroxy-2-(4-iodo-phenyl)-ethyl]-isoindole-1,3-dione | HCID 59331969 | 34% |
反応手順
A mixture of 2-(4-chloro-phenyl)-2-(4-iodo-phenyl)-oxirane* (571 mg, 1.60 mmol) and potassium phthalimide (340 mg, 1.84 mmol) in THF (5 mL) and DMSO (2 mL) was heated at 100° C. for 20 hours. The mixture was concentrated in vacuo, diluted with ethyl acetate and washed with water and brine (×2), dried (MgSO4), filtered and concentrated to give a crude product which was purified by column chromatography (SiO2), eluting with a gradient of ethyl acetate/petrol (2.5% to 100%) then 10% methanol/dichloromethane to give the title compound (273 mg, 34%); LCMS (PS-A2) Rt 3.22 min [M+H]+ 504.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08541461B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-127b327b984c4858890977b1a36ff6a0 |
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| 出典メモ | uspto-grants-2013_09 |
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