反应 #2171082
ord-58aaf6fb93cd4e57894f3b55942ac5a6
反应方程式
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1workup.ADDITIONSilica (3 g) was added
- 2其他volatile material was removed by evaporation
- 3其他The residue was purified by column chromatography
- 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.