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2-Chloroethanol → 2-(5-Iodo-indol-1-yl)-ethanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Chloroethanol | HCID 34 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 5-Iodo-1H-indole | HCID 2782313 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 2-(5-Iodo-indol-1-yl)-ethanol | HCID 45789380 | — |
反応手順
Under an N2 atmosphere 30 g (121 mmol) 5-iodoindole are added to a suspension of 27.1 g (484 mmol) KOH in 150 mL DMSO. The reaction mixture is kept for 1 h at RT, cooled to 0° C. with ice water, 9.7 mL (145 mmol) of 2-chloroethanol in 30 mL DMSO are slowly added dropwise and stirred for 4.5 h at RT. The reaction mixture is combined with 1 L EtOAc, washed four times with in each case 800 mL water and once with 400 mL saturated NaCl solution and the organic phase is dried over Na2SO4. After the desiccant and solvent have been eliminated the residue is purified by chromatography (silica gel, cyc/EtOAc 3:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08618132B2 |
| 出典データセット | uspto-grants-2013_12 |
| ORD ID | ord-6dde589b709a42c683272ae1e51fa024 |
| 出典メモ | uspto-grants-2013_12 |