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Piperazine → o-Phenetidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Piperazine | HCID 4837 | — |
| 反応物 | Isocyanate | HCID 105034 | — |
| 反応物 | 2-bromoethyl-N-(2-ethoxyphenyl)carbamate | HCID 11162014 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | o-Phenetidine | HCID 7203 | — |
反応手順
5 μl of TEA (0.033 mmol, 1.1 eq) is added then 500 μl of piperazine (0.03 mmol, 1 eq) dissolved in DMF to 300 μl of 0.2 M 2-bromoethyl-N-(2-ethoxyphenyl)carbamate (0.06 mmol, 2 eq) dissolved in DMF. After 18 hours at room temperature and evaporation of the solvents, the mixtures are taken up in 1 ml of CH2Cl2 and treated with isocyanate resin (Argonaut, 1.51 mmol/g, 0.09 mmol/g, 0.09 mmol, 3 eq) for 18 hours. Next, the mixtures are purified on cation exchange resins according to the protocol described hereinabove. The desired compounds are then obtained after elimination of the solvents.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07238693B2 |
| 出典データセット | uspto-grants-2007_07 |
| ORD ID | ord-29cfcdddbd9f4490814f1268c90c7ff3 |
| 出典メモ | uspto-grants-2007_07 |