反应 #4301

ord-95c3f93212c34abcafd8589c1a2860f7

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The residue obtained
  2. 2
    萃取the chloroform layer was extracted with water
  3. 3
    干燥The chloroform layer was dried
  4. 4
    过滤filtered
  5. 5
    其他solvent removed
  6. 6
    其他to give a dark brown oil
  7. 7
    其他This salt was recrystallized from methanol-diethyl ether
  8. 8
    其他dried in vacuo overnight at 80° C

实验过程

A solution of 105.95 g (0.456 mole) [(4-chlorobutyl)sulfonyl]benzene was heated overnight at 75° C. on an autoclave in 200 ml of isopropylamine. The reaction mixture was stripped to dryness. The residue obtained was dissolved in chloroform and the chloroform layer was extracted with water. The chloroform layer was dried, filtered, and solvent removed to give a dark brown oil. The oil was dissolved in methanol and converted to the hydrochloride salt. This salt was recrystallized from methanol-diethyl ether and dried in vacuo overnight at 80° C. This gave white crystalline product, m.p. 155°-157.5° C. in 30% yield.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04724235uspto-grants-1988_02