N-(9-Fluorenylmethoxycarbonyloxy)succinimide synthesis
- Product Name:N-(9-Fluorenylmethoxycarbonyloxy)succinimide
- CAS Number:82911-69-1
- Molecular formula:C19H15NO5
- Molecular Weight:337.33
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82911-69-1
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Yield:82911-69-1 56.3%
Reaction Conditions:
with sodium carbonate in water;toluene at 25 - 30; for 2 h;Reagent/catalyst;Solvent;
Steps:
1-3 Example 2:
Into a 1000ml four-necked flask, 100g of water was added, under stirring, 105g of hydroxylamine hydrochloride (molecular weight 164.1, 0.64mol) was added, and 250g of liquid alkali with a mass fraction of 40% (molecular weight 40.0, 2.5mol) was added dropwise. 152.3g of succinic anhydride (molecular weight 100.1, 1.52mol), stir to dissolve completely, add 5g of sulfuric acid with a mass fraction of 98% (molecular weight 98, 0.05mol), vacuum dehydration, control the temperature in the bottle not higher than 160 , to anhydrous Drop out, cool to below 100 , Add 200g of toluene, heat to reflux with stirring, reflux to separate water until no water comes out, drop to 25 30 ,A toluene solution (molecular weight 258.7, 0.89mol) containing 230g of 9-fluorenyl methyl chloroformate was added, and 500g of sodium carbonate aqueous solution (sodium carbonate 47g, water 453g) was added dropwise to the reaction bottle. At this time, the solid in the bottle disappeared and quickly Stirring, dropwise addition, heat preservation for 2 hours, let stand, separate water layer, concentrate organic layer to dryness, add dichloromethane 600g, warm to reflux, drop to room temperature for crystallization, suction filtration, filter cake drying: 240g, Rate: 56.3%, purity determined by HPLC is 99.9%, melting point: 148-150 ° C.
References:
CN110818607,2020,A Location in patent:Paragraph 0011; 0024-0029
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