N,N-DIMETHYLHYDROXYLAMINE HYDROCHLORIDE

N,N-DIMETHYLHYDROXYLAMINE HYDROCHLORIDE 속성

N,N-DIMETHYLHYDROXYLAMINE HYDROCHLORIDE C화학적 특성, 용도, 생산

용도

N,N-Dimethylhydroxylamine hydrochloride was used in the synthesis of 4,4-dimethyl-2,5,5-triphenyl-l.3-dioxa-4-azonia-2-bora-5-boratacyclopentane. It was also used as a polymer-chain terminator.

제조 방법

(a) Preparation of N,N-Dimethyl~(a-phenylethyl)amine Oxide. To a flask containing 11.0 g (0.074 mole) of N,N-dimethyl(a-phenylethyl)amine is added dropwise 18.3 g (0.19 mole) of 35% aqueous hydrogen peroxide, and the mixture is stirred for 11 hr at room temperature. The excess hydrogen peroxide is decomposed by stirring the mixture with 8 sqcm2 clean platinum foil until the evolution of oxygen ceases. Most of the water is removed by distillation at 35 mm Hg, at a bath temperature of 45-55°C. The material that condenses in the dry-ice trichloroethylene trap is saved for recovery in Procedure (b). The residual syrup is diluted with 25 ml of absolute ethanol, and the process is repeated twice while a capillary ni­trogen ebulliator is used. The resulting amine oxide is a viscous syrup and has a slight odor of styrene.
(b) Decomposition of N,N-Dimethyl-(a-phenylethyl)amine Oxide to Ν,Ν-Dimethylhydroxylamine. A 100 ml round bottom flask equipped with a capillary nitrogen inlet, and containing the preceding amine oxide is connected by a large-diameter tube to a condenser set for distillation with two receivers. Each receiver is cooled in a mixture of dry ice and trichlo­roethylene. The system is evacuated to 5 mm, and the flask is immersed in an oil bath at 85°C. The bath temperature is raised slowly to 115°C over a 35-min period, in which time most of the material distilled over. The bath temperature is finally raised to 150°C, in order to complete the (decom­position) distillation process. The residue remaining averages 0.35 g. The distillate in the dry-ice trap here and from Procedure (a) are combined, pentane is added as a solvent, and the mixture is washed with dilute hydrochloric acid. The acid solution is extracted with pentane, the latter washed with water until neutral.
The product is obtained from the combined aqueous layers containing hydrochloric acid by concentration under reduced pressure, to give a crys­talline residue. The latter, upon drying in a vacuum desiccator over P2O5 averages 6.73 g (94% yield), m.p. 101-101°C (sealed capillary). Recrys-tallization several times from a mixture of absolute ethanol and ether gives white, hygroscopic needles, m.p. 106.5-109°C (sealed capillary).

N,N-DIMETHYLHYDROXYLAMINE HYDROCHLORIDE 준비 용품 및 원자재

원자재

준비 용품

N,N-DIMETHYLHYDROXYLAMINE HYDROCHLORIDE 공급 업체

공급자	전화	이메일	국가	제품 수	이점
Shenzhen Nexconn Pharmatechs Ltd	+86-755-89396905 +86-15013857715	admin@nexconn.com	China	10318	58
LEAPCHEM CO., LTD.	+86-852-30606658	market18@leapchem.com	China	43348	58
Shanghai Acmec Biochemical Technology Co., Ltd.	+undefined18621343501	product@acmec-e.com	China	33350	58
Aladdin Scientific	+1-+1(833)-552-7181	sales@aladdinsci.com	United States	52927	58
Henan Fangding Technology Co., LTD	15670369782 15670369782	15670369782@163.com	China	9838	58
Energy Chemical	021-021-58432009 400-005-6266	sales8178@energy-chemical.com	China	44700	61
Syntechem Co.,Ltd		info@syntechem.com	China	12990	57
Bide Pharmatech Ltd.	400-1647117 15221909166	product02@bidepharm.com	China	41438	60
Shanghai Macklin Biochemical Co.,Ltd.	15221275939 15221275939	shenlinxing@macklin.cn	China	16168	55
Jiangsu Aikon Biopharmaceutical R&D co.,Ltd.	025-66113011 18112977050	cb6@aikonchem.com	China	16687	50

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