تفاعل #8177

ord-4f84ead693da4f968cd28a52005d8455

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةat reflux for 30 hours
  2. 2
    ترشيحThe resulting precipitate was collected by filtration
  3. 3
    غسيلwashed thoroughly with water several times
  4. 4
    أخرىair-dried
  5. 5
    أخرىdried under vacuum

الإجراء التجريبي

A stirred solution of 4-chlorobenzenesulfonamide (38.33 g, 200 mmol) and anhydrous hydrazine (31.4 mL, 1.0 mol) was heated at reflux for 30 hours. After cooling to room temperature, the mixture was poured into water (500 mL) with swirling. The resulting precipitate was collected by filtration, washed thoroughly with water several times, air-dried, and dried under vacuum to give the title compound (35.5 g, 95% yield) as a white solid. Mp 169–171° C. 1H NMR (300 MHz, THF-d8) δ 7.59 (d, J=8.8 Hz, 2H), 6.77 (d, J=8.8 Hz, 2H), 6.62 (br, 1H), 5.99 (br, 2H), 3.87 (br, 2H). Mass spectrum (API-TIS) m/z 188 (MH+).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07087630B2uspto-grants-2006_08