تفاعل #5524

معادلة التفاعل

2-amino-6-chloropyridine

ethyl bromopyruvate

→

desired product

المردود 67.7%

2-ethoxycarbonyl-5-chloroimidazo[1,2-a]pyridine

المردود 67.7%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux for 4 hours
2. 2
   أخرىAfter the solvent was removed
3. 3
   workup.ADDITIONchloroform was added to the residue, which
4. 4
   غسيلwas washed in turn with saturated sodium bicarbonate and saturated saline
5. 5
   تجفيفdried over anhydrous magnesium sulfate
6. 6
   تركيزAfter the solvent was concentrated
7. 7
   workup.ADDITIONn-hexane was added to the mixture
8. 8
   أخرىThen, the crystals precipitated
9. 9
   ترشيحwere filtered off
10. 10
    غسيلwashed with n-hexane

الإجراء التجريبي

A solution of 2-amino-6-chloropyridine (6.43 g, 50 mmoles) and ethyl bromopyruvate (9.75 g, 50 mmoles) in ethanol (150 ml) was heated at reflux for 4 hours. After the solvent was removed, chloroform was added to the residue, which was washed in turn with saturated sodium bicarbonate and saturated saline, and then dried over anhydrous magnesium sulfate. After the solvent was concentrated, n-hexane was added to the mixture. Then, the crystals precipitated were filtered off and washed with n-hexane to obtain 7.60 g of the desired product (67.6%, pale yellow crystals).

المصدر