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Hydrogen Bromide → 2-(1,3-Benzodioxol-5-yl)-2-bromoacetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | 3',4'-Methylenedioxymandelic acid | HCID 119618 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(1,3-Benzodioxol-5-yl)-2-bromoacetic acid | HCID 11345950 | — |
反応手順
62% Aqueous hydrobromic acid (220 ml) was added slowly to a stirred suspension of 2-(1,3-benzodioxol-5-yl)-2-hydroxyacetic acid (see J Org Chem, 50(23), 4523-6, 1985; 82.4 g) in a mixture of toluene (500 ml) and dichloromethane (1 liter). The mixture was stirred vigorously for 4 h. The aqueous layer was separated and removed and the organics were dried (MgSO4) and concentrated to give a brown oil. The oil crystallised over a 24 h period to give 105.3 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06211223B1 |
| 出典データセット | uspto-grants-2001_04 |
| ORD ID | ord-ca7941e975254853b7dfc53b89b25352 |
| 出典メモ | uspto-grants-2001_04 |