反应详情

Add 1.15 g (8.9 mmol) DIEA to 1.0 g (3.0 mmol) 4-chloro-5-(4-methoxyphenyl)-6-phenylfuro[2,3-d]pyrimidine and 0.70 g (5.9 mmol) 6-aminohexanol in 10 ml DMF and heat for 4 h to 120° C. Then dilute the mixture with ethyl acetate, wash with water and dilute hydrochloric acid, dry, and concentrate by evaporation. Purify the residue by RP-HPLC (column: Gromsil 250 mm×40 mm, 10 μm; acetonitrile/water gradient: 0-3 min 5% acetonitrile, 3-34 min 5%→98% acetonitrile, 34-38 min 98% acetonitrile). 364 mg (29% of theor.) 6-{[5-(4-methoxyphenyl)-6-phenylfuro[2,3-d]pyrimidin-4-yl]amino}hexan-1-ol is obtained as a yellow oil, which solidifies after standing for 2 days.

1. temperatureheat for 4 h to 120° C
2. washwash with water and dilute hydrochloric acid
3. customdry
4. concentrationconcentrate by evaporation
5. customPurify the residue by RP-HPLC (column: Gromsil 250 mm×40 mm, 10 μm; acetonitrile/water gradient: 0-3 min 5% acetonitrile, 3-34 min 5%→98% acetonitrile, 34-38 min 98% acetonitrile)