반응 #81821

ord-85aae3c011414557809e137dd866b50d

용매

반응 조건

온도
170°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling to room temperature the mixture
  2. 2
    추출extracted with ethyl acetate
  3. 3
    세척The organic phase was washed
  4. 4
    기타dried
  5. 5
    기타evaporated

실험 절차

A suspension of the 2-chloro-5,11-dihydro-11-ethyl-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (0.14 g) in 3-hydroxypyrrolidine (0.29 g) in an open test tube was heated at 170° C. for 30 minutes. After cooling to room temperature the mixture was diluted with water and extracted with ethyl acetate. The organic phase was washed, dried, and evaporated. Chromatography over silica gel with ethyl acetate gave the title compound, which crystallized from ethyl acetate. Yield, 0.12 g, m.p. 131°-134° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05620974uspto-grants-1997_04