3-BROMO-4-HYDROXYDIPHENYL synthesis
- Product Name:3-BROMO-4-HYDROXYDIPHENYL
- CAS Number:92-03-5
- Molecular formula:C12H9BrO
- Molecular Weight:249.1
Yield:92-03-5 92.5%
Reaction Conditions:
with tetrakis(triphenylphosphine) palladium(0);potassium carbonate in ethanol;water;toluene at 90; for 5 h;Inert atmosphere;
Steps:
1.2 Step 2: Preparation of Intermediate 2
Under the protection of nitrogen, dissolve raw material C (50 mmol) and raw material D (55 mmol) in a mixed solution of 150 mL of toluene, 50 mL of ethanol and 50 mL of water, add tetrakistriphenylphosphine palladium (0.5 mmol) and potassium carbonate (100 mmol), and stir well , Warm up to 90°C and reflux for 5 hours. After the solution is cooled to room temperature, keep the organic phase, and then extract the aqueous phase with 100 mL of ethyl acetate; after combining the organic phases, use anhydrous magnesium sulfate for drying, and use rotary evaporation The solvent is removed by the device to obtain solid organic matter. Use 30mL of dichloromethane to completely dissolve the solid organic matter, then slowly add dropwise to the petroleum ether solution, stir evenly, precipitate precipitation, suction filtration to obtain the solid, followed by rinsing with 300mL of absolute ethanol, 200mL of petroleum ether, and drying to obtain Intermediate 2 (11.52 g, yield 92.5%, MW: 249.15).
References:
CN112812123, 2021, A Location in patent:Paragraph 0058; 0060; 0063-0064
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