反应详情

温度

70 °C

To a suspension of 2.9 g. (0.12 mole) of sodium hydride in oil were added 13 g. (0.035 mole) of 2-(4-methoxyphenyl)-3-(4-methoxybenzoyl)benzothiophene (prepared as in Example 13) dissolved in DMF. The resulting mixture then was added to a cold solution of DMF containing 7.5 g. of ethyl mercaptan. The mixture was stirred at 70° C. for two hours and was monitored by TLC until little or no starting material remained. The total reaction time was about two hours. The mixture then was concentrated to dryness, water was added, and the aqueous mixture was acidified and extracted with ethyl acetate. The ethyl acetate extract was washed, dried over magnesium sulfate, and evaporated to a residue. The residue was recrystallized from benzene to obtain 9.1 g. (73 percent) of 2-(4-methoxyphenyl)-3-(4-hydroxybenzyl)benzothiophene, melting point 188°-189° C.

1. additionTo a suspension of 2.9 g
2. waitThe total reaction time was about two hours
3. concentrationThe mixture then was concentrated to dryness, water
4. additionwas added
5. extractionextracted with ethyl acetate
6. extractionThe ethyl acetate extract
7. washwas washed
8. dry with materialdried over magnesium sulfate
9. customevaporated to a residue
10. customThe residue was recrystallized from benzene
11. customto obtain 9.1 g