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ChemicalBook CAS DataBase List FW 358.2
5701-82-6

FW 358.2 synthesis

9synthesis methods
-

Yield: 88.25%

Reaction Conditions:

with trifluoroacetic acid;HSiPh3 in dichloromethane at 20; for 48.5 h;Inert atmosphere;Reagent/catalyst;Temperature;

Steps:

3-5 Example 4: Synthesis of 1,4-bis(3,4-dimethoxyphenyl)-2,3-dimethylbutane
Dissolve 20 grams (51 mmol) of 1,4-bis(3,4-dimethoxyphenyl)-2,3-dimethyl-2,3-butanediol white solid in 200mL of anhydrous dichloromethane , Add 58.20 g (37.9 mL, 510 mmol) of trifluoroacetic acid, add 30.47 g (117 mmol) of triphenylsilane in 200 mL of anhydrous dichloromethane solution dropwise at room temperature under nitrogen protection. The dripping time takes about 30 minutes. The dripping is complete. React at room temperature for 48 hours. After the reaction is complete, the reaction product is poured into 500 mL of saturated sodium bicarbonate solution. The aqueous layer is extracted with 250 mL of dichloromethane. The organic layers are combined and washed with 200 mL of saturated sodium bicarbonate solution. The organic layer is concentrated to dryness under reduced pressure. , Recrystallized with absolute ethanol to obtain 16.13 g of crystal product, yield 88.25percent, melting point 93-94°C.

References:

Jincheng Tiancheng Kechuang Co., Ltd.;Su Guiping CN111205171, 2020, A Location in patent:Paragraph 0027-0038