반응 #1996

ord-e9a35b5778f84e018ef46a7daf51dbfd

반응 방정식

CCOC(=O)c1cc(C2CC2)c2c(C)c(C3(C(=O)O)CC3)c(F)cn2c1=O
product
CCOC(=O)c1cc(C2CC2)c2c(C)c(C3(C(=O)O)CC3)c(F)cn2c1=O
1-cyclopropyl-8-(1-hydroxycarbonyl-1-cyclopropyl)-7-fluoro-9-methyl-4-oxo-4H-quinolizine-3-carboxylic acid ethyl ester
[N-]=[N+]=NP(=O)(c1ccccc1)c1ccccc1
diphenylphosphoryl azide
CC(C)(C)O
t-butanol
CCN(CC)CC
triethylamine
CCOC(=O)c1cc(C2CC2)c2c(C)c(C3(NC(=O)OC(C)(C)C)CC3)c(F)cn2c1=O
1-cyclopropyl-8-(1-Bocamino-1-cyclopropyl)-7-fluoro-9-methyl-4-oxo-4H-quinolizine-3-carboxylic acid ethyl ester

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvents is removed under vacuum
  2. 2
    workup.DISSOLUTIONThe residue is dissolved in methylene chloride
  3. 3
    세척washed with water
  4. 4
    건조dried over MgSO4
  5. 5
    농축concentrated under vacuum
  6. 6
    기타The title compound is purified by chromatography on silica gel

실험 절차

A sample of the product from Step 477d is heated with diphenylphosphoryl azide, t-butanol, triethylamine and dioxane. The solvents is removed under vacuum. The residue is dissolved in methylene chloride, washed with water and dried over MgSO4 and concentrated under vacuum. The title compound is purified by chromatography on silica gel.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05726182uspto-grants-1998_03