Tetrakis(dimethylphosphoniumbismethylide)dinickel, a New Type of Cage Compound

✍ Scribed by Dipl.-Chem Hans Heinz Karsch; Prof. Dr. Hubert Schmidbaur

• Publisher: John Wiley and Sons
• Year: 1973
• Tongue: English
• Weight: 213 KB
• Volume: 12
• Category: Article
• ISSN: 0044-8249
• DOI: 10.1002/anie.197308531

✦ Synopsis

C~~~Iolir.~trrircarbaldehpdc atid cw-bmzoylbeiizyl cjriohrx-at~ecurbos~~latr Cyclohexene (250g, 3.05mol), benzil (250g, 1.19mol), and R h 2 0 3 (0.10 g) are placed in a 2-1 steel autoclave previously purged with nitrogen and are heated at 120 C with synthesis gas (20 atm cold pressure). The synthesis gas pressure is raised from 25 to 30 atm during the reaction. After 11 hours' reaction, distillation of the autoclave content affords cyclohexanecarbaldehyde (146 g) boiling at 5&56 "C/17 torr and a-benzoylbenzyl cyclohexanecarboxylate (308 g, 80% yield based on benzil), boiling at 175-177"C/0.2 torr, m.p. 100-101 "C (from light petroleum).