Boron tribromide → Ethyl 5-hydroxybenzofuran-2-carboxylate
反応式
[CH2:1]([O:3][C:4]([C:6]1[O:7][C:8]2[CH:14]=[CH:13][C:12]([O:15]C)=[CH:11][C:9]=2[CH:10]=1)=[O:5])[CH3:2].B(Br)(Br)Br>C(Cl)Cl>[CH2:1]([O:3][C:4]([C:6]1[O:7][C:8]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][C:9]=2[CH:10]=1)=[O:5])[CH3:2]参加物
4
反応条件
- 温度
- 0 °C
実験手順
The above prepared 5-methoxy-benzofuran-2-carboxylic acid ethyl ester (8.10 g, 36.8 mmol) was dissolved in 250 mL of CH2Cl2, cooled to 0° C., and treated with BBr3 (73.6 mL of 1M solution in CH2Cl2, 2 eq.). After 2 h, the reaction mixture was carefully poured onto crashed ice, twofold extracted with CH2Cl2, washed with brine, dried over magnesium sulfate, and evaporated to dryness. Ensuing flash chromatography (SiO2, hexane/AcOEt=8/2) delivered then 5.63 g of the title compound as off-white crystals.
後処理
- additionthe reaction mixture was carefully poured
- extractiontwofold extracted with CH2Cl2
- washwashed with brine
- dry with materialdried over magnesium sulfate
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-fae4dd29020d4c56ba37b03c148f2d48
- 出典データセット
- uspto-grants-2009_05
- 特許番号
- US07534788B2
反応ノート
読み込み中…