Acetic Anhydride → 142034-81-9

To a cooled solution of trans-2-carboxymethoxy-cyclohexyl ammonium chloride (1.048 g, 5 mmoles) in 2N NaOH (5 ml), there were added under stirring first 1N NaOH (1 ml) and then acetic anhydride (0.102 g, 1 mmol). When the reaction of anhydride was completed and a homogeneous solution was obtained, the same amount of 1N NaOH and acetic anhydride as above was added four times. After the addition of the last portion the reaction mixture was stirred for 30 minutes, the solution was acidified to pH 2 and extracted with ethyl acetate (5×20 ml). The organic extracts were dried with MgSO4, the drying agent was filtered off and the filtrate was evaporated under reduced pressure. The residue was recrystallized from a mixture of chloroform/n-hexane. Thus, there were obtained 0.60 g (56%) of the title compound, melting point 141°-143° C.

1. customa homogeneous solution was obtained
2. additionAfter the addition of the last portion the reaction mixture
3. extractionextracted with ethyl acetate (5×20 ml)
4. dry with materialThe organic extracts were dried with MgSO4
5. filtrationthe drying agent was filtered off
6. customthe filtrate was evaporated under reduced pressure
7. customThe residue was recrystallized from a mixture of chloroform/n-hexane

ORDレコード

ord-7bf474be29824fc6b0a9a3d97dcb6ff5

出典データセット

uspto-grants-1993_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05231216