반응 #2186206

반응 방정식

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

POCl3

sodium bicarbonate

→

crude product

수율 66.0%

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

수율 66.0%

용매

DMF

반응 조건

후처리

1. 1
   온도cooled below 10° C
2. 2
   온도heated to 90° C. for 30 minutes
3. 3
   온도to cool to 30° C.
4. 4
   추출The desired product is extracted with ethyl acetate and saline
5. 5
   건조the organic phase dried over sodium sulfate
6. 6
   기타evaporated

실험 절차

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.

출처