تفاعل #4496

معادلة التفاعل

cyclohexanethiocarboxamide

ethyl 4-chloroacetoacetate

→

ethyl 2-cyclohexyl-4-thiazoleacetate

المردود 71.3%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةunder reflux for 1 hour
3. 3
   استخلاصAfter dilution with water, mixture was extracted with ethyl acetate
4. 4
   غسيلThe extract was washed with aqueous sodium bicarbonate solution and water
5. 5
   تجفيفdried (MgSO4)
6. 6
   تركيزconcentrated
7. 7
   أخرىThe residue was purified by chromatography on silica gel with ethyl acetate-hexane (1:4)

الإجراء التجريبي

A mixture of cyclohexanethiocarboxamide (5.0 g), ethyl 4-chloroacetoacetate (5.74 g), ethanol (50 ml) was heated under reflux for 1 hour. After dilution with water, mixture was extracted with ethyl acetate. The extract was washed with aqueous sodium bicarbonate solution and water, dried (MgSO4), and concentrated. The residue was purified by chromatography on silica gel with ethyl acetate-hexane (1:4) to yield ethyl 2-cyclohexyl-4-thiazoleacetate as an oil (6.3 g, 70.9%). IR (Neat): 1735, 1255 cm-1. NMR (CDCl3)δ: 1.28 (3H, t, J=7 Hz), 1.2-2.3 (10H, m), 2.97 (1H, m), 3.77 (2H, s), 4.17 (2H, q, J=7 Hz), 7.0 (1H, s).

المصدر