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Ethanolamine → 1-(4-Chloro-phenyl)-2-(2-hydroxy-ethylamino)-1-(4-iodo-phenyl)-ethanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanolamine | HCID 700 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-(4-Chlorophenyl)-2-(4-iodophenyl)oxirane | HCID 59317217 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 1-(4-Chloro-phenyl)-2-(2-hydroxy-ethylamino)-1-(4-iodo-phenyl)-ethanol | HCID 59331967 | 99.9% |
反応手順
A solution of 2-(4-chloro-phenyl)-2-(4-iodo-phenyl)-oxirane (0.60 g, 1.68 mmol), ethanolamine (0.5 mL, 8.3 mmol) and triethylamine (0.5 mL, 3.6 mmol) in iso-propanol (5 mL) was maintained at 50° C. for 72 hours then concentrated in vacuo. The residue was taken up in ethyl acetate and washed with saturated potassium carbonate solution/water (1:9). The aqueous phase was extracted a second time with ethyl acetate, then the combined extracts were washed with brine, dried (MgSO4), filtered and concentrated to give the title compound (701 mg, quantitative); LCMS (PS-A2) Rt 2.29 min [M+H]+ 418, [M−H2O+H]+ 400.
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 |
| ORD ID | ord-974860b0b1ac4481b8f2061acf6e8a2c |
| 出典メモ | uspto-grants-2013_09 |