Hydrochloride methanol → HCID 67315093, compound

Participants

Reaction Steps

7.2 g of unpurified 4-[(4-dipropylaminobutyl)amino]methylbenzylamine (5a) synthesized in Example 12 was diluted with 20 ml of methanol. 32.9 g (3.6 equivalents) of a 10% hydrochloric acid-methanol solution was added dropwise to the mixture under cooling with ice. The mixture was stirred for one hour at a same temperature, and then concentrated. Hexane was added to the residue obtained, and the resulting mixture was azeotropically distillated. This operation was repeated three times to completely remove methanol, thereby obtaining white crystals. The crystals were dissolved in 120 ml of a mixed solvent (IPA:MeOH=3:1) at 70° C. The solution was stirred overnight at room temperature to precipitate white crystals. The crystals were filtered and dried under reduced pressure, thereby obtaining 7.81 g of 4-[(4-dipropylaminobutyl)amino]methylbenzylamine hydrochloride (5aa) (yield: 74.9%). m. p. 205 to 210° C.

Provenance & Evidence