Formaldehyde → HCID 22070441, compound

Participants

Reaction Steps

10.0 g of N,N-Di(3-Anisyl)amine were dissolved 436 ml of anhydrous THF. 14.0 g of paraformaldehyde were added with stirring followed by 8.20 g of sodium borohydride. 190 ml of trifluoro acetic acid were added during 120 min and after completion of the addition the reaction mixture was stirred at room temperature over night. The reaction mixture was poured into 654 ml of an ice cubes containing 25.0%-weight solution of sodium hydroxide in water. After addition of 654 ml of a saturated aqueous solution of sodium chloride it was extracted three times with each 650 ml of dichloromethane and the combined organic extracts were dried with anhydrous sodium sulfate. After filtration the solvent was removed in vacuo and the crude product purified by fractionated distillation in vacuo. At a temperature of 125-135° C./0.04 mbar 8.60 g (80.4%) of DAMA are collected as yellow liquid.

Provenance & Evidence