4-Formylbenzoic acid → 4-Formylbenzoyl chloride
反応式
[Cl-].[Cl:2]C=[N+](C)C.[C:7]([C:10]1[CH:17]=[CH:16][C:13]([CH:14]=[O:15])=[CH:12][CH:11]=1)(O)=[O:8]>C(Cl)Cl>[CH:14]([C:13]1[CH:16]=[CH:17][C:10]([C:7]([Cl:2])=[O:8])=[CH:11][CH:12]=1)=[O:15]参加物
4
反応条件
- 温度
- 0 °C
実験手順
A suspension of (chloromethylene)dimethylammonium chloride (Vilsmeier Reagent; 37.7 g, 0.280 mol) in CH2Cl2 (300 mL) at 0° C. was treated with 4-carboxybenzaldehyde (40.0 g, 267 mmol) in one portion. The reaction mixture was stirred at 0° C. for 30 min, then at room temperature for 2 h. HPLC analysis of an aliquot of the reaction mixture quenched into MeOH indicated consumption of 4-carboxybenzaldehyde. The reaction mixture was filtered through a medium porosity glass frit. The filtrate, containing the title compound, was stored at 0° C., and used in the next step without further manipulation.
後処理
- waitat room temperature for 2 h
- customHPLC analysis of an aliquot of the reaction mixture quenched into MeOH
- customconsumption of 4-carboxybenzaldehyde
- filtrationThe reaction mixture was filtered through a medium porosity glass frit
- additionThe filtrate, containing the title compound
- customwas stored at 0° C.
出典と根拠
- ORDレコード
- ord-a6cfdb8f7041403d96a62694f8d57739
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07728129B2
反応ノート
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