Process for preparing di-tert-butyl dicarbonate of high purity

Abstract

This invention discloses a process for preparing high-purity di-tert-butyl dicarbonate, relating to the field of biopharmaceutical manufacturing technology. The method includes using coconut shell activated carbon as raw material, which is deashed, etched, oxidized, and grafted with amino groups to obtain an amino-functionalized mesoporous activated carbon support; dissolving anhydrous aluminum trichloride, anhydrous magnesium chloride, and anhydrous ferric chloride, adding acetylacetone, oxalic acid, and polyethylene glycol-400, and then adding the resulting solution to the support for coordination anchoring, thus preparing a multi-metal coordination-anchored supported catalyst; using this catalyst to catalyze the reaction of metallic sodium with anhydrous tert-butanol to prepare a sodium tert-butoxide solution; subsequently, a low-temperature carbonylation reaction and an esterification reaction are performed to obtain a crude di-tert-butyl dicarbonate solution; the crude solution is then subjected to low-temperature quenching, washing, drying, low-temperature vacuum distillation, and programmed temperature recrystallization to obtain high-purity di-tert-butyl dicarbonate. This invention produces ultra-high-purity di-tert-butyl dicarbonate, meeting the needs of high-end applications.

Images