90609-89-5|4-Methoxy-3-methylbenzaldehyde oxime| Ambeed

Yield	Reaction Conditions	Operation in experiment
	With ammonium acetate;palladium on activated charcoal; In methanol; for 18.0h;	Intermediate (ii) fr3-methvl-4- (methvloxv) phenvllmethvlamine To Intermediate intermediate (i) (1 equiv. ) in MeOH (200mL) at rt is added [MeCO2] NH4 (6 equiv. ), Pd/C (0.01 equiv. ) and molecular sieves The reaction is then heated to reflux for 18h. The reaction mix is filtered through celite, evaporated to dryness and treated with HCI (1N). The aqueous layer is washed with CH2CI2, filtered, basified to pH > 14 and extracted with CH2CI2 (3 x 50mL). The combined organic layers are washed with H2O, dried over Na2SO4, filtered and evaporated to dryness to afford the title compound as an oil
	With sodium tetrahydroborate; titanium tetrachloride; In 1,2-dimethoxyethane; at 0 - 20℃;	[3-methyl-4-(methyloxy)phenyl]methyl}amine hydrochloride4-methoxy-3-methylbenzaldehyde (10g, 66.6mmol), hydroxylamine hydrochloride (7.87g,111. 2mmol) and Et3N (63ml, 440mmol) inCH2CI2 (250ml) were stirred at rt for 18h. The mixture was quenched with water (150ml), the aqueous phase extracted withCH2CI2(150mi) andethylacetate (150ml). The organic layers were evaporated to give the product A. To a solution of 10.6 g(280mol) of NaBH4 in 150 mL of anhydrous DME under argon at0 C was added dropwise TiCl4 (15.3moi,140mol) then the product A diluted in 50 mL of DME was added dropwise maintaining temperature at0 C. The resulting mixture was stirred at rt overnight. At0 C, the mixture was quenched with a progressive addition of 200 mL of water, then basified with NaOH (25%) A dark blue precipitate formed. The organic layer was extracted <Desc/Clms Page number 83>three times with ethyl acetate, filtered and evaporated. The resulting yellow oil was diluted in anhydrous diethyl ether and, at0 C, 50 mL of HCI (2N in diethyl ether) was added to give a white precipitate which was filtered off (10.9g). Yield : 87% 'H NMR (DMSO)6 : 7.33-7. 24 (m, 2H); 6.95 (d, 1H); 3.88 (m, 2H); 3.78 (s, 3H); 2.14 (s, 3H)

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H420	Harms public health and the environment by destroying ozone in the upper atmosphere

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CAS No.: 90609-89-5

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CAS No.: 90609-89-5

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