반응 #794572

ord-690c6f22928242ca9603ac729cabfe09

용매

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Reaction mixture
  2. 2
    온도was heated to 85° C. for 3 hr
  3. 3
    기타at 110° C.
  4. 4
    기타overnight
  5. 5
    기타Reaction mixture
  6. 6
    세척washed with water and brine
  7. 7
    기타Purification by Biotage (0-10% MeOH/DCM)
  8. 8
    기타produced product

실험 절차

To a solution of cis-3-(((benzyloxy)carbonyl)amino)cyclobutyl 4-methylbenzenesulfonate (0.563 g, 1.5 mmol) in DMF (3.00 ml) was added 2H-pyrido[3,2-b][1,4]oxazin-3(4H)-one (FSSI, 0.225 g, 1.500 mmol) and potassium carbonate (EMD, 0.415 g, 3.00 mmol). The resulting mixture was heated to 50° C. overnight. Reaction mixture was heated to 85° C. for 3 hr then at 110° C. overnight. Reaction mixture was diluted with DCM and washed with water and brine. Purification by Biotage (0-10% MeOH/DCM) produced product. Material was advanced to the next step. M+1: 353.9

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09174992B2uspto-grants-2015_11