反应 #46301

ord-14ae93f0e2fc4239bc147c2f8b2320e3

反应方程式

COc1c2c(c3n(c1=O)CCC(O)CN(C)C3=O)CCN(Cc1ccc(F)c(Cl)c1)C2=O
11-(3-chloro-4-fluorobenzyl)-4-hydroxy-9-methoxy-2-methyl-3,4,5,6,12,13-hexahydro-2H[1,4]diazocino[2,1-a]-2,6-naphthyridine-1,8,10(11H)-trione
C[N+]1([O-])CCOCC1
N-methylmorpholine N-oxide
COc1c2c(c3n(c1=O)CCC(=O)CN(C)C3=O)CCN(Cc1ccc(F)c(Cl)c1)C2=O
title compound
COc1c2c(c3n(c1=O)CCC(=O)CN(C)C3=O)CCN(Cc1ccc(F)c(Cl)c1)C2=O
11-(3-Chloro-4-fluorobenzyl)-9-methoxy-2-methyl-5,6,12,13-tetrahydro-2H[1,4]diazocino[2,1-a]-2,6-naphthyridine-1,4,8,10(3H, 11H)-tetrone

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The mixture was filtered
  2. 2
    浓缩the filtrate concentrated under vacuum
  3. 3
    其他Collection and concentration of appropriate fractions

实验过程

A mixture of 11-(3-chloro-4-fluorobenzyl)-4-hydroxy-9-methoxy-2-methyl-3,4,5,6,12,13-hexahydro-2H[1,4]diazocino[2,1-a]-2,6-naphthyridine-1,8,10(11H)-trione (50 mg, 0.11 mmol), molecular sieves (4A), N-methylmorpholine N-oxide (19 mg, 0.16 mmol), and tetra-n-propylammonium ruthenium tetroxide in dichloromethane was stirred at room temperature for two hrs. The mixture was filtered, and the filtrate concentrated under vacuum. The residue was subjected to column chromatography on silica gel eluting with 0-15% methanol in dichloromethane gradient. Collection and concentration of appropriate fractions provided the title compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07741315B2uspto-grants-2010_06