2-Bromo-9,9-dimethylfluorene synthesis
- Product Name:2-Bromo-9,9-dimethylfluorene
- CAS Number:28320-31-2
- Molecular formula:C15H13Br
- Molecular Weight:273.17
Yield:28320-31-2 98%
Reaction Conditions:
Stage #1: 2-Bromofluorenewith benzyl-triethyl-ammonium chloride;sodium hydroxide in lithium hydroxide monohydrate;dimethyl sulfoxide at 20; for 0.333333 h;Inert atmosphere;
Stage #2: iodomethane in lithium hydroxide monohydrate;dimethyl sulfoxide; for 4 h;Inert atmosphere;
Steps:
1.S1 S1: make the compound of formula (1) undergo methylation reaction to generate the compound of formula (2):
This step is specifically: at room temperature, in a 200mL single-neck round-bottom flask,Add 1 g of the compound of formula (1) and 20 mL of dimethyl sulfoxide,Then 2 ml of 50% aqueous sodium hydroxide solution and 50 mg of TEBAC were added to the system,After stirring for 20 min, 0.9 g of methyl iodide was added, and stirring was continued for 4 h;Quenched with water, extracted with dichloromethane, dried over anhydrous magnesium sulfate, and distilled under reduced pressure to remove the solvent;The crude product was purified by column chromatography (eluent: petroleum ether) to obtain 1.1 g of the compound of formula (2) as a white solid with a yield of 98%.
References:
CN114249746,2022,A Location in patent:Paragraph 0039; 0043-0045
4569-45-3
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28320-31-2
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