関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cyclopentanol | HCID 7298 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | (s)-(4-Nitro-benzenesulfonylamino)-phenyl-acetic acid | HCID 362697 | — |
| 生成物 | (S)-(4-Nitro-benzenesulfonylamino)-phenyl-acetic acid cyclopentyl ester | HCID 57971706 | 70% |
反応手順
To a solution of stage 1 acid (4.32 g, 12.8 mmol) in cyclopentanol (60 ml) at 0° C. was added slowly thionyl chloride (9.3 ml, 128 mmol). The reaction mixture was stirred and heated under reflux at 70° C. for 2 hours. The excess thionyl chloride was removed by evaporation in vacuo, the reaction mixture was extracted into EtOAc and washed with saturated NaHCO3 solution and dried over Na2SO4, filtered and evaporated to dryness. Flash column chromatography purification with DCM gave the required product (3.6 g, 70% yield). LCMS purity of 100%, (molecular ion not observed).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07939666B2 |
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| 出典データセット | uspto-grants-2011_05 |
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| ORD ID | ord-d55b19ec942c4fa399650079061003a9 |
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| 出典メモ | uspto-grants-2011_05 |
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