Oxidations hydrochloride

Methyl-4-nitropyridine-l-oxide has been prepared by the nitration of 3-methylpyridine-l-oxide hydrochloride with a mixture of concentrated sulfuric acid and potassium nitrate. The I)reparation of this compound has been mentioned briefly by Talikowa, but no experimental details have been given. 

Chemical Name 7-chloro-N-methyl-5-phenvl-3H-1,4-benzodiazepin-2-amino-4-oxide hydrochloride... 

To a warm solution (50°C) of 172.5 g (0.7 mol) of 2-amino-5-chlorobenzophenone-o -oxime in one liter glacial acetic acid were added 110 cc (1.47 mols) chloroacetyl chloride. The mixture was heated for 10 minutes at 50°C and then stirred at room temeprature for 15 hours. The precipitated yellow prisms, 2-chloromethyl-4-phenyl-6-chloroquinazoline 3-oxide hydrochloride, were filtered off, melting range 128° to 150°C with dec. 

Ninety-eight grams of 6-chloro-2-chloromethyl-4-phenylquinazoline 3-oxide hydrochloride were introduced into 600 cc of ice cold 25% methanolic methylamine. The mixture was initially cooled to about 30°C and then stirred at room temperature. After 15 hours the reaction product which precipitated was filtered off. The mother liquor was concentrated in vacuo to dryness. The residue was dissolved in methylene chloride, washed with water and dried with sodium sulfate. The methylene chloride solution was concentrated in vacuo and the crystalline residue was boiled with a small amount of acetone to dissolve the more soluble impurities. The mixture was then cooled at 5°C for 10 hours and filtered. The crystalline product, 7-chloro-2-methylamino-5-phenyl-3H-1,4-benzodiazepine 4-oxide, was recrystallized from ethanol forming light yellow plates, MP 236° to 236.5°C. 

A. Pyridine-N-oxide hydrochloride. The acetate is converted to the hydrochloride by bubbling a slight excess over the thcoret-... 

For Negishi reactions in which the pyridines are nucleophiles, the pyridylzinc reagents are usually prepared from the corresponding halopyridines [6, 20, 21]. An excess of 2-chlorozincpyridine /V-oxide (26), arising from 2-bromopyridine N-oxide hydrochloride (25), was coupled with vinyl triflate 27 in the presence of Pd(Ph3p)4 to furnish adduct 28 [20]. Recently, an efficient Pd-catalyzed cyanation of 2-amino-5-bromo-6-methylpyridine (29) using zinc cyanide has been reported to afford pyridyl nitrile 30 [22]. 

DLs for impurities should correspond to less than 0.1% of the main compound " compounds that take effect in lower amounts may require lower DLs. For example, imipramine N-oxide hydrochloride impurities and salicylamide impurities have been determined at the 0.01% level. DLs and QLs in CE are generally to some extent higher (in concentration) than in HPLC because of the small optical path (50—100 pm) used for ultraviolet (UV) detection and small injected volume (2—20nl) compared with HPLC 10 mm optical length and 10—200 pi injected volume. ... 

Furaltadone 332.9 Methdilazine Hydrochloride 341.8 Atropine Oxide Hydrochloride... 

Atropine methobromide, 365 Atropine methonitrate, 365 Atropine methylbromide, 365 Atropine oxide, 365 Atropine oxide hydrochloride, 365 Atropine sulpha.te, 364 Atropinol, 363 Atropisol, 364 Atropt, 364... 

Amin Bis-[2-chlor-ethyl]-methyl- -oxid (Hydrochlorid) XI/2, 197... 

CFA750 CAS 302-70-5 HR 3 2-CHLORO-N-(2-CHLOROETHYL)-N-METHYLETHANAMINE-N-OXIDE HYDROCHLORIDE... 

CHLORDIAZEPOXIDE MONOHYDROCHLORIDE CHLORIDEAZEPOXIDE HYDROCHLORIDE 7-CHL-ORO-2-METHYLAMINO-5-PHEN YD3H-1,4-BENZODI-AZEPIN, 4-OXIDE, HYDROCHLORIDE 7-CHLORO-N-METHYL-5-PHENYL-EH-l,4-BENZODIAZEPIN-2-AMINE-4-OXIDE, MONOHYDROCHLORIDE CORAX... 

CHLORO-2-METHYLAMINO-5-PHENYL-3H-l,4-BENZODIAZEPINE 4-OXIDE see LFKOOO 7-CHLORO-2-METHYLAAnNO-5-PHENYL-3H-l,4-BENZODIAZEPIN 4-OXIDE see LFKOOO 7-CHLORO-2-METHYLAAnNO-5-PHENYL-3H-l,4-BENZODIAZEPIN, 4-OXIDE, HYDROCHLORIDE see MDQ250... 

DICHLORO-N-METHYLDIETHYLAMINE N-OXIDE HYDROCHLORIDE see CFA750 N-(DICHLOROMETHYLENE)ANTLINE see PFJ400 4,4 -DICHLORO-2,2 -METHYLENEDIPHENOL see... 

MECHLORETHAMINE OXIDE see CFA500 MECHLORETHAMINE OXIDE HYDROCHLORIDE see CFA750... 

N-METHYLBIS(2-CHLOROETHYL)AMINE-N-OXIDE HYDROCHLORIDE see CFA750 METHYLBIS(P-CHLOROETHYL)xAVnNE-N-OXIDE HYDROCHLORIDE see CFA750... 

The nitrile or ester is heated under reflux with concentrated hydrochloric acid (20-25 ml per gram of substrate) for 4h. The iV-oxide hydrochloride which separates from the cooled solution is recrystallizcd, then decomposed by dissolving it in aqueous ammonia (d. 0.88 40ml per gram of hydrochloride), and tire solution is concentrated at 50°C under reduced pressure until Crystallization commences. After cooling, the A -oxidcs are filtered. 

Chlordiazepoxide hydrochloride is 7-chloro-2-(methylamino)-5-phenyl-3H-l,4-benzodiazepine 4-oxide hydrochloride. 

Chlor-2,3-dihydro- -4-oxid 1343 2.3-Dihydro- -4-oxid 1343 6-Nilro-2,3-dihydro- -4-oxid-Hydrochlorid 1343... 

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