반응 #698629

ord-50b4ea20d9b148bca48d75e7c2081bce

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The solution was cooled
  2. 2
    기타solid formed
  3. 3
    여과The mixture was filtered
  4. 4
    세척the solid was washed with diethyl ether
  5. 5
    기타recrystallized from ethanol

실험 절차

A solution of [4-(6-methoxy-benzothiazol-2-ylazo)phenyl]-dimethyl-amine (Example 4b, 0.75 g, 2.40 mmol) and dimethyl sulfate (0.50 mL, 5.28 mmol) in 15 mL of chlorobenzene was heated under nitrogen at 70° C. for 3 hours. The solution was cooled and solid formed. The mixture was filtered, the solid was washed with diethyl ether and recrystallized from ethanol to give the title compound as a dark blue-black solid, mp 206-207° C., dec.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06001331uspto-grants-1999_12