反応 #308290

反応方程式

thiazole

iodobenzene

potassium acetate

→

5-phenylthiazole

溶媒

N,N-dimethylacetamide

反応条件

後処理

1. 1
   その他The solvent was evaporated under reduced pressure
2. 2
   workup.ADDITIONadded to the residue
3. 3
   洗浄The mixture was washed successively with water and brine
4. 4
   乾燥dried over sodium sulfate
5. 5
   その他The solvent was evaporated under reduced pressure
6. 6
   その他the residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0-90:10)

実験手順

A solution of thiazole (10.0 g), iodobenzene (2.63 ml), tetrakis(triphenylphosphine)palladium (0) (1.36 g) and potassium acetate (3.46 g) in N,N-dimethylacetamide (100 ml) was stirred under heating at 100° C. overnight. The solvent was evaporated under reduced pressure, and added to the residue was ethyl acetate. The mixture was washed successively with water and brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0-90:10) to give 5-phenylthiazole (1.50 g) as a pale yellow solid. APCI-Mass m/Z 162 (M+H). (2) The above 5-phenylthiazole and 5-bromo-2-chlorobenzaldehyde obtained in Reference Example 16-(1) were treated in a manner similar to Reference Example 100 to give 5-bromo-2-chloro-1-(5-phenyl-2-thiazolylmethyl)benzene as a yellow solid. APCI-Mass m/Z 364/366 (M+H).

出典