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ChemicalBook CAS DataBase List 3,4,5-TRICHLOROPHENOL

3,4,5-TRICHLOROPHENOL synthesis

8synthesis methods
-

Yield:609-19-8 49%

Reaction Conditions:

with copper(I) oxide;copper(II) nitrate in water at 20; for 1.16667 h;

Steps:

54

Add solid 3,4, 5-trichloro benzenediazonium tetrafluoroborate. (9.62 g, 32.6 mmol, 1 equiv. ) to a room temperature solution of copper (II) nitrate trihydrate (450 g, 1.86 mol, 57 equiv. ) and copper (I) oxide (14.03 g, 98.1 mmol, 3 equiv. ) in water (3.5 L) and vigorously stir the reaction mixture at room temperature for lhlOmin. The solids are filtered and then washed with dichloromethane. Extract the filtrate three times with dichloromethane, dry over anhydrous magnesium sulfate, filter, and concentrate under reduced pressure. Purify on silica gel eluting with 0 to 20% EtOAc/hexanes to give the title compound as an orange brown solid (3.199 g, 49%).'H NMR (CDC13) 8 6.91 (s, 2H), 4. 95 (br s, 1H).

References:

WO2005/92835,2005,A1 Location in patent:Page/Page column 38

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