تفاعل #5740

ord-5b876d1b98bf447b958335604e70efcd

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe mixture was removed from the cooling bath
  2. 2
    درجة الحرارةcooled to 0° C.
  3. 3
    workup.ADDITION65 mL ice cold hexanes was added
  4. 4
    ترشيحThe white precipitate was collected by filtration
  5. 5
    غسيلwashed two times with a small amount of cold hexanes
  6. 6
    أخرىdried in vacuo

الإجراء التجريبي

A solution of methanol (10.2 mL, 252 mmoles) in 15 mL toluene was added dropwise to a solution of chlorosulfonyl isocyanate (22.0 mL, 252 mmoles) in 75 mL toluene at 0° C. The mixture was removed from the cooling bath and stirred for one-half hour at room temperature, then cooled to 0° C. and 65 mL ice cold hexanes was added. The white precipitate was collected by filtration and washed two times with a small amount of cold hexanes and dried in vacuo to give 33.0 g of a white solid, mp 72°-74° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05245068uspto-grants-1993_09