関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Formylbenzoic acid | HCID 12088 | — |
| 反応物 | Chloro-N,N-dimethylformiminium chloride | HCID 77311 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Formylbenzoyl chloride | HCID 12424620 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07728129B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-a6cfdb8f7041403d96a62694f8d57739 |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|
