反应详情

温度

25 °C

32.6 gm (0.2 mol) of 6-hydroxy-3,4-dihydro-carbostyril [see F. F. Mayer et al., Ber. Dtsch. Chem. Ges. 60, 858 (1927)] and 27.6 gm (0.2 mol) of potassium carbonate were stirred for 5 minutes in 600 ml of dimethylsulfoxide which had been dried over a molecular sieve, and then 52.2 gm of 4-phenylsulfinyl-butyl bromide (0.2 mol) (prepared from thiophenol and 1,4-dibromo-butane and subsequent oxidation with hydrogen peroxide in glacial acetic acid analogous to Example 2; oily substance, solidified upon standing in the refrigerator) were added. After stirring it for 15 hours at 25° C., the reaction mixture was poured into 6 liters of water. After stirring the aqueous mixture for 30 minutes more, the precipitated product was suction-filtered off and thoroughly washed with water. After drying, the filter cake was recrystallized from about 600 ml of xylene in the presence of charcoal. White crystals with a melting point of 144.5°-145.5° C. were obtained.

1. customhad been dried over a molecular sieve
2. additionwere added
3. stirringAfter stirring the aqueous mixture for 30 minutes more
4. filtrationthe precipitated product was suction-filtered off
5. washthoroughly washed with water
6. customAfter drying
7. customthe filter cake was recrystallized from about 600 ml of xylene in the presence of charcoal
8. customWhite crystals with a melting point of 144.5°-145.5° C. were obtained