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Tributylamine → 2-Amino-5-bromo-3-iodobenzenesulphonyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tributylamine | HCID 7622 | — |
| 反応物 | Triphenylphosphine dichloride | HCID 260420 | — |
| 反応物 | 2-Amino-5-bromo-3-iodobenzenesulphonic acid | HCID 18919385 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Amino-5-bromo-3-iodobenzenesulphonyl chloride | HCID 18931670 | — |
反応手順
To a solution containing 7.6 g (20 mmol) of 2-amino-5-bromo-3-iodobenzenesulphonic acid and 4.8 ml (20 mmol) of tributylamine in 20 ml of dichloromethane is added dropwise, at 0° C. under a nitrogen atmosphere, a solution of dichlorotriphenylphosphorane (9.7 g (37.5 mmol) in 45 ml of dichloromethane). The mixture is brought to room temperature, stirring is continued for 18 hours and the product is purified by chromatography on a column of silica gel, eluting with a dichloromethane/pentane mixture (2:8).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05739382 |
| 出典データセット | uspto-grants-1998_04 |
| ORD ID | ord-7ceb11856b154c8fbd018051b434b437 |
| 出典メモ | uspto-grants-1998_04 |