تفاعل #4301

ord-95c3f93212c34abcafd8589c1a2860f7

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe residue obtained
  2. 2
    استخلاصthe chloroform layer was extracted with water
  3. 3
    تجفيفThe chloroform layer was dried
  4. 4
    ترشيحfiltered
  5. 5
    أخرىsolvent removed
  6. 6
    أخرىto give a dark brown oil
  7. 7
    أخرىThis salt was recrystallized from methanol-diethyl ether
  8. 8
    أخرىdried in vacuo overnight at 80° C

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04724235uspto-grants-1988_02