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3,4:5,6-Di[1,3]butadieno-9H-fluorene synthesis

3synthesis methods
-

Yield:194-58-1 99%

Reaction Conditions:

with hydrazine hydrate;potassium hydroxide in diethylene glycol at 170; for 3 h;

Steps:

1.1-3 Preparation Example 1-3: Preparation of 7H-dibenzo[c,g]fluorene

The solution, in which 7H-dibenzo[c,g]fluoren-7-one (641 mg, 2.29 mmol), N2H4.H2O (2.86 g, 57.2 mmol) prepared in the Preparation Example 1-2 and KOH (385 mg, 6.86 mmol) were dispersed in diethylene glycol (30 mL), was stirred at 170° C. for 3 hours. The reaction was terminated by adding 10% HCl at 0° C. and the resulting solid was filtered. Drying under vacuum gave 603 mg (99%) of 7H-dibenzo[c,g]fluorine, which is a dark brown solid compound having the following 1H-NMR spectrum.
1H-NMR (CDCl3, 300 MHz): δ 8.73 (d, 2H), 7.97 (d, 2H), 7.86 (d, 2H), 7.73 (d, 2H), 7.59-7.48 (m, 4H), 4.13 (s, 2H).

References:

US2021/171559,2021,A1 Location in patent:Paragraph 0054-0055