반응 #413873

ord-c4aecccb27b64080b91bc05032c6deae

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture became quite warm
  2. 2
    기타a heavy white precipitate formed
  3. 3
    workup.STIRRINGThe reaction mixture was stirred an additional 15 minutes
  4. 4
    여과the precipitate was recovered by filtration

실험 절차

A solution of 6.25 g (49.00 mmoles) of 4-chloroaniline in 10 ml of methylene chloride was added to a solution of 9.85 g (49.95 mmoles) of p-toluenesulfonyl isocyanate in 75 ml of methylene chloride with stirring. The mixture became quite warm and a heavy white precipitate formed. An additional 100 ml of methylene chloride were added. The reaction mixture was stirred an additional 15 minutes, and the precipitate was recovered by filtration affording 15.0 g of the title product as a white solid. A small amount of the material was crystallized from diethyl ether to provide the title compound (87% yield) with a melting point of 174-176° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05270329uspto-grants-1993_12