تفاعل #67278

معادلة التفاعل

1-[5-bromo-3-fluoro-2-(oxiran-2-ylmethoxy)phenyl]ethanone

m-CPBA

m-CPBA

→

crude title compound

المردود 189.4%

5-BROMO-3-FLUORO-2-(OXIRAN-2-YLMETHOXY)PHENYL ACETATE

المردود 189.4%

المذيبات

DCM

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux
2. 2
   درجة الحرارةthe mixture was heated
3. 3
   درجة الحرارةat reflux for another 22 h
4. 4
   أخرىbrought to ambient temperature
5. 5
   ترشيحThe solid was filtered off
6. 6
   غسيلrinsed
7. 7
   غسيلThe resulting filtrate was washed with sodium bicarbonate (saturated), brine
8. 8
   تجفيفfurther dried (Na2SO4)
9. 9
   أخرىevaporated to dryness

الإجراء التجريبي

A solution of 1-[5-bromo-3-fluoro-2-(oxiran-2-ylmethoxy)phenyl]ethanone (1.3 g, 4.5 mmol) and m-CPBA (4.0 g, 18 mmol) in DCM (25 ml) was heated at reflux. After 22 h more m-CPBA (2.7 g, 12 mmol) was added and the mixture was heated at reflux for another 22 h and then brought to ambient temperature. The solid was filtered off and rinsed. The resulting filtrate was washed with sodium bicarbonate (saturated), brine and further dried (Na2SO4) and evaporated to dryness to give the crude title compound (2.6 g). MS m/z (rel. intensity, 70 eV) 305 (M+, 5), 304 (M+, 6), 263 (97), 262 (bp), 206 (49), 57 (65).

المصدر