反应详情

4-amino-2,6-diethyl-3-iodopyridine (2 g) (obtained as described in Example 7 B) was added to a mixture of potassium t-butoxide (0.97 g) and 1,4,7,10,13,16-hexacyclooctadecane (200 mg) in THF (40 ml) and the mixture was stirred for 15 minutes. Compound E (4 g) was added and the mixture was stirred for 4 hours. Volatile material was removed by evaporation and the residue was dissolved in dichloromethane. The solution was washed with 0.1M citric acid solution and dried (MgSO4). Solvent was removed by evaporation and the residue was purified by flash chromatography eluting with dichloromethane/methanol (12:1 v/v) to give 2,6-diethyl-3-iodo-4-[(2'-(1-(4-nitrophenyl)-1H-tetrazol-5-yl)biphenyl-4-yl)methylamino]pyridine (F) (0.9 g) as a solid; NMR (CDCl3): 1.26(d of t, 6H), 2.70(q, 2H), 3.00(q, 2H), 4.35(d, 2H), 5.21(broad t, 1H), 6.10(s, 1H), 6.58(d, 2H), 6.79(d, 2H), 7.04(d, 2H), 7.37(m, 1H), 7.65(m, 2H), 7.86(d, 3H).

1. stirringthe mixture was stirred for 4 hours
2. customVolatile material was removed by evaporation
3. dissolutionthe residue was dissolved in dichloromethane
4. washThe solution was washed with 0.1M citric acid solution
5. dry with materialdried (MgSO4)
6. customSolvent was removed by evaporation
7. customthe residue was purified by flash chromatography
8. washeluting with dichloromethane/methanol (12:1 v/v)