Diisopropylethylamine → HCID 21446145, compound

Participants

Reaction Steps

4.8 g (0.0178 mole) of 1'-(3-chloropropionyl)-spiro[bicyclo[2.2.2]octane-2,3'-piperidine] is dissolved in 50 ml of abs. benzene; an addition is then made of 3.0 g (0.018 mole) of (1RS, 2RS, 4SR)-spiro[norbornane-2,3'-piperidine] (see Example 2) and 3.5 g (0.0267 mole) of diisopropylethylamine, and the whole refluxed in a nitrogen atomosphere, with stirring, for 42 hours. The mixture is concentrated in vacuo under 12 Torr, and the residue distributed between 50 ml each of water and of chloroform. After separation of the chloroform extract, the aqueous phase is subsequently extracted again with 50 ml of chloroform. The chloroform extracts are washed separately twice with 50 ml of water each time; they are then dried over sodium sulphate and concentrated in vacuo (ca. 12 Torr). There is thus obtained crude 1'-[3-(1RS,2RS,4SR)-spiro[norbornane-2,3'-piperidin]-1' -yl)-propionyl]-spiro[bicyclo[2.2.2]octane-2,3'-piperidine] as colourless oil.

Provenance & Evidence