ChemicalBook CAS DataBase List 1-(4-methoxyphenyl)-2-(methylamino)ethanone hydrochloride

1-(4-methoxyphenyl)-2-(methylamino)ethanone hydrochloride synthesis

4synthesis methods

Product Name:1-(4-methoxyphenyl)-2-(methylamino)ethanone hydrochloride
CAS Number:29705-80-4
Molecular formula:C10H13NO2
Molecular Weight:179.22

A solution of a-bromo-4-methoxyacetophenone in acetonitrile was added to a solution of dimethylamine (8 M solution in ethanol) in acetonitrile at 0°. The solution was stirred at 0° for 5 min. Ether was added and the resulting precipitate after drying, was dissolved in ether and 1 M hydrogen chloride in ether was added at 0°.

74-89-5 Synthesis

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1-(4-methoxyphenyl)-2-(methylamino)ethanone hydrochloride

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Yield:29705-80-4 59%

Reaction Conditions:

Stage #1: methylamine;p-methoxyphenacyl bromide in dichloromethane;acetonitrile at -30; for 0.166667 h;
Stage #2: with hydrogenchloride in lithium hydroxide monohydrate;ethyl acetate; for 0.0833333 h;

Steps:

1 Synthesis of 1- (4-methoxyphenyl) -2- (methylamino) ethanone hydrochloride (2)

In a 1000 mL reaction flask, acetonitrile (200 mL) was added, and a 30% solution of methylamine (104 mL, 0.68 mol) was added at -30 ° C,Bromoethanone 1 (31.00 g, 0.14 mol) was dissolved in acetonitrile (150 mL)Add dichloromethane (50mL) to help dissolve, the constant pressure dropping funnel slowly dripped, the reaction was completed 10min,The reaction was complete by TLC.Dichloromethane (350 mL) was added and the mixture was washed with cold, saturated sodium bicarbonate, cold water and brine, and the organic phase was dried over anhydrous sodium sulfate. The filtrate was filtered, the filtrate was added 1.125mol / L hydrochloric acid ethyl acetate solution (239mL, 0.27mol), stirred 5min, desolventizing, with an appropriate amount of acetone was washed and suction filtered to give a white solid 17.14g, yield 59%.

References:

CN107304185,2017,A Location in patent:Paragraph 0038; 0039; 0040; 0041;