ChemicalBook CAS DataBase List 3-Bromo-9,9-dimethylfluorene

3-Bromo-9,9-dimethylfluorene synthesis

5synthesis methods

Product Name:3-Bromo-9,9-dimethylfluorene
CAS Number:1190360-23-6
Molecular formula:C15H13Br
Molecular Weight:273.17

2038-91-7 Synthesis

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Yield:1190360-23-6 96%

Reaction Conditions:

with sodium t-butanolate in dimethyl sulfoxide at 80 - 90; for 0.5 h;

Steps:

3-bromo-9,9-dimethyl-9H-fluorene

37 g (152 mmol) of 3-bromo-9H-fluorene are dissolved in 600 ml of dry DMSO in a flask dried by heating. 43.9 g (457 mmol) of NaOtBu are added at room temperature. Let the blue suspension now have an internal temperature of 80 ° C. At this temperature, 64.8 g (457 mmol) of iodomethane are added dropwise to the purplish solution at a rate that does not exceed an internal temperature of 90 deg. C (duration: about 30 minutes). The batch is kept at an internal temperature of 80-90 ° C for an additional 30 minutes, then poured into 1500 ml of ice water and stirred for about 20 minutes. The precipitated solid is filtered off with suction and washed successively with about 200 ml of H2O and methanol. Yield: 39 g (144 mmol), 96% of theory; Purity: 95% by'H-NMR.

References:

KR2017/59015,2017,A Location in patent:Paragraph 0229-0231