反应 #2171082

ord-58aaf6fb93cd4e57894f3b55942ac5a6

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONSilica (3 g) was added
  2. 2
    其他volatile material was removed by evaporation
  3. 3
    其他The residue was purified by column chromatography
  4. 4
    洗涤eluting with 0-40% ethyl acetate/isohexane

实验过程

A solution of 2,4-dichloropyrimidine (596 mg, 4.0 mmol), indoline (0.45 ml, 4.0 mmol) and N,N-diisopropylethylamine (0.69 ml, 4.0 mmol) in n-butanol (20 ml) was heated at 100° C. for 18 hours. Silica (3 g) was added and volatile material was removed by evaporation. The residue was purified by column chromatography, eluting with 0-40% ethyl acetate/isohexane, to give the product as a colourless solid (460 mg, 50%). NMR (CDCl3): 3.2 (t, 2H), 4.0-4.1 (t, 2H), 6.5 (d, 1H), 7.0-7.1 (m, 1H) 7.2-7.3 (m, 2H), 8.2 (m, 1H), 8.3-8.4 (m, 1H); MS (MH+): 232.7.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06716831B1uspto-grants-2004_04