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Water → Methyl 2-amino-2-(2-iodophenyl)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Azido-(2-iodophenyl)-acetic Acid Methyl Ester | HCID 86632577 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 2-amino-2-(2-iodophenyl)acetate | HCID 68840368 | — |
反応手順
To a solution of azido-(2-iodophenyl)-acetic acid methyl ester in THF (100 mL) is added triphenylphosphine (28.5 g, 109 mmol) in portions. The mixture is stirred at RT for 2 h then water (4 mL) is added and is heated to reflux. The solvent is removed under reduced pressure and ether (50 mL) is added followed by 2N HCl until acidic. The aqueous phase is washed with methylene chloride then is concentrated and basified with NaOH/ice until pH 12. The mixture is extracted with methylene chloride (3×200 mL) and the combined organic phases are dried over sodium sulfate. The solvent is removed under reduced pressure to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08084448B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-3fdcbc5ba307497db4a744a835fe307d |
| 出典メモ | uspto-grants-2011_12 |