HRID1263100

反应详情

EQUATION

反应方程式

HRID 1263100 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

120 Milliliters of γ-chlorobutyryl chloride and 160 g of pulverized anhydrous aluminium chloride were suspended in 300 ml of carbon disulfide. The suspension was refluxed by heating and another suspension of 29.4 g of 3,4-dihydrocarbostyril in 100 ml of carbon disulfide was added dropwise to the first suspension in 1 hour and the reaction was continued for 4 hours under refluxing condition by heating. After the reaction was completed, the reaction mixture was poured into ice-water and the precipitates thus formed were collected by filtration, washed with water and with ether. Then the washed precipitates were recrystallized from acetone to obtain 25.5 g of 6-(4-chloro-1-oxobutyl)-3,4-dihydrocarbostyril in yellow needle-like crystals. Melting point: 158°-160° C.

WORKUP

后处理

  1. temperatureThe suspension was refluxed
  2. temperatureby heating
  3. additionwas added dropwise to the first suspension in 1 hour
  4. temperatureunder refluxing condition
  5. temperatureby heating
  6. customthe precipitates thus
  7. customformed
  8. filtrationwere collected by filtration
  9. washwashed with water and with ether
  10. customThen the washed precipitates
  11. customwere recrystallized from acetone