반응 #1472089

ord-331e9ad355244fa5b174c6e3dd15994d

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The obtained mixture was heated
  2. 2
    온도under reflux
  3. 3
    workup.WAITAfter several hours
  4. 4
    농축the reaction mixture was concentrated under a reduced pressure
  5. 5
    workup.ADDITIONfollowed by the addition of water
  6. 6
    기타The crystal thus precipitated
  7. 7
    여과was recovered by filtration
  8. 8
    세척washed with water
  9. 9
    기타air-dried

실험 절차

5.00 g (17.3 mmol) of 2,4-dichloro-6,7,8-trimethoxyquinazoline was suspended in 100 ml of methanol, followed by the gradual addition of 1.5 g of sodium hydride. The obtained mixture was heated under reflux. After several hours, the reaction mixture was concentrated under a reduced pressure, followed by the addition of water. The crystal thus precipitated was recovered by filtration, washed with water and air-dried to give 4.80 g of the title compound as a pale-pink crystal.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06262059B1uspto-grants-2001_07