Sodium Hydroxide → HCID 86621004, compound

Participants

Reaction Conditions

Reaction Steps

10g (29.35 mmol; 1 eq) of sulfonic acid from Example 6b are suspended in 400 ml of tetrahydrofuran in a 500 ml flask, and 11.74 g (293.5 mmol; 10 eq) of sodium hydroxide are subsequently added. The reaction mixture is heated under reflux for 10 h, cooled and acidified, and the sulfonic acid is separated off from the aqueous phase by repeated extraction with methyl t-butyl ether. The organic phase is subsequently washed and evaporated to dryness. The crude sulfonic acid is suspended in 100 ml of ethanol, 1.4 g (35.22 mmol; 1.2 eq) of sodium hydroxide are added, and the mixture is heated at 97° C. for 1 h. After the suspension has been cooled, crystals deposit, which are filtered off and dried.

Provenance & Evidence