ChemicalBook CAS DataBase List HYDROXYLAMINE

HYDROXYLAMINE synthesis

11synthesis methods

Product Name:HYDROXYLAMINE
CAS Number:7803-49-8
Molecular formula:H3NO
Molecular Weight:33.03

Hydroxylamine is unstable as a free base. It is prepared from hydroxy-lamine hydrochloride, NH2OH?HCl, which is obtained by electrolytic reduc-tion of ammonium chloride solution. The hydrochloride undergoes alkalinedecomposition to hydroxylamine, which is collected by vacuum distillation.

5470-11-1 Synthesis

5470-11-1
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7803-49-8
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Yield:-

Reaction Conditions:

with sodium hydroxide in methanol at 5 - 30; for 0.5 h;

Steps:

1.1.c

A solution of sodium hydroxide (3. 31 g, 55.2 mmol) in methanol (30 mL) was added to a hot solution of hydroxylamine hydrochloride (3.83 g, 55.2 mmol) in methanol (30 mL). The mixture was kept under stirring at 25-30 °C for 30 minutes and then cooled to 5-10 °C. The precipitate was removed by filtration. This freshly prepared solution of the hydroxylamine was added to 2- 3-amino-3- [4- (2-methoxymethyl-quinolin-4-ylmethoxy)-phenyl]-2-oxo- pyrrolidin-l-yl}-4-methyl-pentanoic acid methyl ester (1.4 g, 2.76 mmol) obtained above in methanol (10 mL) at 5-10 °C. The mixture was stirred at 25-30 °C for 2 h. and acidified to pH 6.0-6. 5 with 1 N HC1. The hydroxamic acid was precipitated out. The desired 2- {3-amino-3- [4- (2-methoxymethyl-quinohn-4-ylmethoxy)-phenyl]-2-oxo-pyrrolidin-l-yl}-4-methyl- pentanoic acid hydroxyamide was collected by filtration, washed with water (2 x 10 mL) and dried under vacuum to give the compound of formula (1) (1.0 g, 69.5 %).

References:

WO2005/77937,2005,A1 Location in patent:Page/Page column 20