反应详情

温度

0 °C

3-Dimethylamino-1,2-propanediol (6.0 g, 50 mmol) was weighed into a 1 L round bottomed flask with a stir bar. The flask was sealed, flushed with argon, charged with pyridine and cooled to 0° C. 4,4′-Dimethoxytrityl chloride (17.9 g, 1.05 equiv.) was weighed into a 100 mL round bottomed flask, sealed and then dissolved in pyridine (80 mL). The 4,4′-dimethoxytrityl chloride solution was transferred to the stirring reaction mixture slowly, using additional fresh pyridine (20 mL) to effect the transfer of residual 4,4′-dimethoxytrityl chloride. The reaction was allowed to come to room temperature while stirring overnight. The reaction was concentrated in vacuo and re-dissolved in dichloromethane (300 mL). The organic phase was washed with saturated bicarbonate (2×200 mL) and brine (1×200 mL), dried over MgSO4, filtered, concentrated and dried under high vacuum to afford 22.19 g of a yellow gum that was used without further purification.

1. customThe flask was sealed
2. customflushed with argon
3. additioncharged with pyridine
4. customsealed
5. customto come to room temperature
6. concentrationThe reaction was concentrated in vacuo
7. dissolutionre-dissolved in dichloromethane (300 mL)
8. washThe organic phase was washed with saturated bicarbonate (2×200 mL) and brine (1×200 mL)
9. dry with materialdried over MgSO4
10. filtrationfiltered
11. concentrationconcentrated
12. customdried under high vacuum