102774-86-7Relevant articles and documents
Production and cogeneration N [...] succinimide, N '-di-succinimide-based carbon ester method
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Paragraph 0036-0041, (2017/02/09)
The invention belongs to the field of fine chemical engineering, and particularly relates to a method for producing fluorenylmethoxycarbonylacyl succinimide and coproducing N,N'-disuccinimidocarbonate. The method comprises the following steps: (1) preparation of Fmoc-cl: adding THF (tetrahydrofuran), 9-fluorenylmethanol and an organic amine catalyst into a reaction kettle, cooling to 0-10 DEG C, adding solid phosgene, and completely reacting; (2) preparation of Fmoc-Osu and DSC: adding Hosu, cooling to -5 to +5 DEG C, dropwisely adding a tributyl amine tetrahydrofuran solution, heating to room temperature, and completely reacting; (3) filtering to obtain a DSC crude product; and (4) carrying out mother solution after-treatment to obtain the Fmoc-Osu. A proper amount of 9-fluorenylmethanol is added into the Hosu/solid phosgene/tributyl amine system to quantitatively generate the two products Fmoc-Osu and DSC, wherein the DSC precipitates in the form of crystalline solid, and the Fmoc-Osu and tributyl amine hydrochloride are still dissolved in the tetrahydrofuran solvent; and therefore, the two products can be respectively subjected to filtration, purification and other routine operations to obtain the refined products with the purity of greater than 99%.