反応 #2186206

反応方程式

3-[(2-Fluoro-ethyl)-methyl-amino]-phenol

POCl3

sodium bicarbonate

→

crude product

収率 66.0%

4-[(2-Fluoro-ethyl)-methyl-amino]-2-hydroxy-benzaldehyde

収率 66.0%

溶媒

DMF

反応条件

後処理

1. 1
   温度cooled below 10° C
2. 2
   温度heated to 90° C. for 30 minutes
3. 3
   温度to cool to 30° C.
4. 4
   抽出The desired product is extracted with ethyl acetate and saline
5. 5
   乾燥the organic phase dried over sodium sulfate
6. 6
   その他evaporated

実験手順

169 mg (1 mmol) 3-[(2-Fluoro-ethyl)-methyl-amino]-phenol are dissolved in 4 mL DMF and cooled below 10° C. 0.101 mL (1.1 eq.) POCl3 are added dropwise over the course of one minute, the reaction mixture is stirred 10 minutes at room temperature, then heated to 90° C. for 30 minutes. The reaction mixture is allowed to cool to 30° C. and cautiously treated with a slow addition of 8 mL saturated aqueous sodium bicarbonate solution. The desired product is extracted with ethyl acetate and saline, the organic phase dried over sodium sulfate and evaporated to yield 130 mg (66%) crude product as a slightly brownish oil. This compound is used without further purification.

出典