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Approaches to 1H-Cyclopropa[l]phenanthrenes. Eliminations with 1a,9b-Dihydro-1H-cyclopropa[l]phenanthrene Derivatives

✍ Scribed by Paul Müller; Huong Can Nguyen Thi; Jean Pfyffer


Book ID
102858192
Publisher
John Wiley and Sons
Year
1986
Tongue
German
Weight
626 KB
Volume
69
Category
Article
ISSN
0018-019X

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✦ Synopsis


  1. Reaction of 6e and 6f with PhSeH and Pyridine. Selenoxide 6e (9.53 mg) in CH2C12 (1 ml) was reacted with PhSeH (100 mg, 0.6 mmol) and pyridine (10 pl, ca. 0.1 mmol) for 70 h at r.t. The soln. was evaporated and the residue purified by column chromatography (silica gel, CHCI,) to yield 6.6 mg of6b.

The same procedure with selenone 6e (6.3 mg) afforded 2.4 mg of 6b.

  1. Reduction of 3b. To lithium naphthalenide prepared from naphthalene (0.46 g, 3.6 mmol) and Li (0.02 g, 3.6 mmol) in HMPA (5.0 ml) [23], a soh. of 3b (0.6 mmol) in furan (80 ml) was added at -70". The soh. was stirred 3 hat -70", then 5 hat -50" and 10 h a t r.t. After decomposition with EtOH (2.0 ml) at o", the mixture was worked up as usual. Two successive purifications by flash chromatography (silica gel, AcOEt, then CHCl,/hexane 1 :lo) afforded 2d (26%) [7] and 15 (22%) [4], both identified by comparison of their 'H-NMR with those reported.

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