Purification of 4'-chloro-4-biphenylcarboxaldehyde and bisulfite adduct
Described is a method for purifying 4'-chloro-4- biphenylcarboxaldehyde, which comprises reacting 4'-chloro-4- biphenylcarboxaldehyde with sodium bisulfite to obtain the bisulfite adduct of formula (I). The reaction is conducted in an aqueous/acetonitrile solution having an acetonitrile co...
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Zusammenfassung: | Described is a method for purifying 4'-chloro-4- biphenylcarboxaldehyde, which comprises reacting 4'-chloro-4- biphenylcarboxaldehyde with sodium bisulfite to obtain the bisulfite adduct of formula (I). The reaction is conducted in an aqueous/acetonitrile solution having an acetonitrile concentration sufficient to cause the bisulfite adduct to precipitate. The preferred purification process comprises (i) reacting 4'-chloro-4-biphenylcarboxaldehyde with sodium bisulfite in an aqueous/acetonitrile solution having an acetonitrile concentration sufficient to cause the bisulfite adduct to precipitate, (ii) isolating the bisulfite adduct precipitate from the solution, (iii) mixing the isolated bisulfite adduct in an aqueous/acetonitrile solution having a water concentration sufficient to cause the regenerated aldehyde to precipitate and (iv) converting the bisulfite adduct to 4'-chloro-4- biphenylcarboxaldehyde.
Opísaný je spôsob čistenia 4'-chlór-4-bifenylkarboxaldehydu, ktorý zahrnuje reakciu 4'-chlór-4-bifenylkarboxaldehydu s hydrogensiričitanom sodným na získanie hydrogensiričitanového aduktu vzorca (I), pričom reakcia sa uskutočňuje vo vodnom/acetonitrilovom roztoku, ktorý má koncentráciu acetonitrilu dostatočnú na spôsobenie precipitácie hydrogensiričitanového aduktu. Vo výhodnom uskutočnení zahrnuje spôsob čistenia (i) reakciu 4'-chlór-4-bifenylkarboxaldehydu s hydrogensiričitanom sodným vo vodnom/acetonitrilovom roztoku, ktorý má koncentráciu acetonitrilu dostatočnú na spôsobenie precipitácie hydrogensiričitanového aduktu; (ii) izoláciu precipitátu hydrogensiričitanového aduktu z roztoku; (iii) miešanie izolovaného hydrogensiričitanového aduktu vo vodnom/acetonitrilovom roztoku, ktorý má koncentráciu vody dostatočnú na spôsobenie precipitácie regenerovaného aldehydu a (iv) premenu hydrogensiričitanového aduktu na 4'-chlór-4- bifenylkarboxaldehyd. |
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