Ammonia → HCID 19099826, compound

Participants

Reaction Steps

The compound of Example 56 (9.72 g, 0.031 mole) was mixed with tetrahydrofuran (60 ml), Raney-Cobalt (2.8 g) and ammonia (12 g, 0.706 mole) in a 360 ml Hastelloy-C Shaker tube. The tube was pressurized with hydrogen to 500 psi at room temperature. The tube was then heated at 110° C. for 18 hrs while the hydrogen pressure was adjusted to 1500 psi under the reaction process. The product mixture was filtered first, then was distilled to give the desired product 4.3 g as a clear, colorless liquid. Bp 85° C./0.02 mmHg. H-1 NMR (CDCl3): 3.98 (s, br, 2H), 2.76 (t, J=6 Hz, 4H), 1.80-1.50 (m, 8H), 1.30 (s, br, 4H); F-19 NMR (CDCl3): -81.1 (s, 6F).

Provenance & Evidence