反应详情

温度

65 °C

THF (15 ml) was added to 2-Chlorotrityl chloride resin (4.0 g, 1.2 mmol/g) and the mixture was agitated for 25 min. FmocN(Bn)CH2CH2OCH2CH2OH (6.1 g, 14.7 mmol) in THF (25 ml) was added followed by pyridine (850 μl, 10.5 mmol) and the mixture was heated to 65° C. for 15 h. MeOH (5 ml) was added and heating was continued for 35 min. The resin was filtered, washed with DMF (3×), CH2Cl2 (3×). MeOH (3×) and Et2O (3×) to give 5.0 g. A small sample was dried carefully and deprotected with DCM/piperidine (1:1) for 30 min. Photometric determination of the resulting Fmoc-piperidine adduct (absorption at 301 nm) gave a resin loading of 0.45 mmol/g.

1. temperatureheating
2. waitwas continued for 35 min
3. filtrationThe resin was filtered
4. washwashed with DMF (3×), CH2Cl2 (3×)
5. customMeOH (3×) and Et2O (3×) to give 5.0 g
6. customA small sample was dried carefully
7. waitdeprotected with DCM/piperidine (1:1) for 30 min