反应详情

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0 °C

A suspension of N-[(9H-fluoren-9-ylmethoxy)carbonyl]hydrazine (141) (1.49 g, 5.78 mmol), CH2Cl2 (60 ml) and saturated NaHCO3 solution (60 ml) was stirred vigorously at 0° C. for 5 minutes, and the solution was then left for 5 minutes without stirring. Phosgene (1.89 M in toluene, 7.95 ml, 15.0 mmol) was then carefully added to the lower, organic phase using a syringe, and stirring of the reaction mixture was begun again immediately after the addition. After 10 minutes, water (20 ml) and CH2Cl2 (20 ml) were added to the reaction mixture. The phases were then separated rapidly, the aqueous phase was extracted with CH2Cl2 (50 ml), and the combined organic phases were dried over Na2SO4. Removal of the solvent under reduced pressure and drying gave a colourless solid (1.35 g, 4.82 mmol, 83%).

1. waitthe solution was then left for 5 minutes
2. stirringwithout stirring
3. stirringstirring of the reaction mixture
4. additionafter the addition
5. waitAfter 10 minutes
6. customThe phases were then separated rapidly
7. extractionthe aqueous phase was extracted with CH2Cl2 (50 ml)
8. dry with materialthe combined organic phases were dried over Na2SO4
9. customRemoval of the solvent under reduced pressure
10. customdrying