تفاعل #816410

معادلة التفاعل

product

4-Bromo-3-thiophene-formamide

tributylstannyl(trimethylsilyl)acetylene

→

4-(trimethylsilyl)ethinyl-3-thiophene formamide

المردود 27.7%

ظروف التفاعل

المعالجة

1. 1
   أخرىinto degassed toluene (20 ml)
2. 2
   درجة الحرارةthe mixture was heated
3. 3
   درجة الحرارةunder reflux for 16 hours under an atmosphere of nitrogen
4. 4
   درجة الحرارةAfter cooling
5. 5
   أخرىthe solvent was removed
6. 6
   أخرىthe residue was chromatographed on silica gel (hexane:ethylacetate 3:1)
7. 7
   أخرىAfter three consecutive crystallisations from hexane

الإجراء التجريبي

The product from step B (1 g), tributylstannyl(trimethylsilyl)acetylene (2.16 g) and palladium(tetrakis)triphenylphoshine (0.28 g) were placed into degassed toluene (20 ml) and the mixture was heated under reflux for 16 hours under an atmosphere of nitrogen. After cooling, the solvent was removed and the residue was chromatographed on silica gel (hexane:ethylacetate 3:1). After three consecutive crystallisations from hexane, 0.3 g of 4-(trimethylsilyl)ethinyl-3-thiophene formamide was obtained (m.p. 90-94° C.).

المصدر