反応 #94590

反応方程式

hydrochloric acid

2-Hydroxy-5-ethylbenzoyl chloride

2-methylthiophene

→

title product

(2-Hydroxy-5-ethylphenyl)(5-methyl-2-thienyl)methanone

溶媒

tetrachloroethane

tetrachloroethane

反応条件

後処理

1. 1
   その他being at about 20° C.
2. 2
   温度by cooling with an ice bath
3. 3
   workup.STIRRINGThe mixture was then stirred at room temperature for 3 hours
4. 4
   workup.WAITleft
5. 5
   抽出extracted with chloroform
6. 6
   抽出The chloroform extract
7. 7
   洗浄was washed firstly with a saturated solution of sodium bicarbonate and secondly with a saturated solution of sodium chloride
8. 8
   乾燥was dried (over Na2SO4)
9. 9
   ろ過filtered
10. 10
    その他evaporated
11. 11
    その他to leave an oil which
12. 12
    workup.DISTILLATIONdistilled

実験手順

2-Hydroxy-5-ethylbenzoyl chloride (6.08g, 0.036 mol) and 2-methylthiophene were mixed together in tetrachloroethane (20 ml), and stannic chloride (18.78g, 0.072 mol) in tetrachloroethane (20 ml) was added dropwise with stirring, the temperature of the mixture being at about 20° C. by cooling with an ice bath. The mixture was then stirred at room temperature for 3 hours and left to stand at room temperature overnight. The resulting pink solution was poured into ice and concentrated hydrochloric acid (10 to 20 ml), stirred until the ice had melted and extracted with chloroform. The chloroform extract was washed firstly with a saturated solution of sodium bicarbonate and secondly with a saturated solution of sodium chloride, was dried (over Na2SO4), filtered and evaporated to leave an oil which distilled to give the pure title product (4.36g), bp 133°-136° C./0.1 mm, nD21 1.6341.

出典