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ChemicalBook CAS DataBase List BISNORCHOLENALDEHYDE
3986-89-8

BISNORCHOLENALDEHYDE synthesis

5synthesis methods
-

Yield:3986-89-8 98%

Reaction Conditions:

with 1-hydroxy-3H-benz[d][1,2]iodoxole-1,3-dione in tetrahydrofuran;dimethyl sulfoxide at 20; for 5 h;Reagent/catalyst;Temperature;Solvent;

Steps:

1.1-1; 1.1-2

(1-2) Add BA (5.0g, 15.13mmol) in a 250mL single-necked flask,IBX (8.5 g, 30.26 mmol), 50 mL THF and 50 mL DMSO, react at room temperature for 5 hours.After the reaction was detected by TLC, water was added, filtered with suction, and extracted with dichloromethane (50mL×3).Wash with water (50mL×2), saturated sodium bicarbonate solution (50mL), dry with anhydrous sodium sulfate,Concentration under reduced pressure, purification by silica gel column chromatography (PE/EA=3/1, v/v),Compound 2 (4.9 g, white solid, molar yield 98%) was obtained.

References:

CN111560045,2020,A Location in patent:Paragraph 0047-0049

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