ChemicalBook CAS DataBase List 2-Hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone

2-Hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone synthesis

6synthesis methods

Product Name:2-Hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone
CAS Number:106797-53-9
Molecular formula:C12H16O4
Molecular Weight:224.25

1-Propanone, 1-[4-(2-hydroxyethoxy)phenyl]-2-methyl-

159119-01-4

2-Hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone

106797-53-9

The general procedure for the synthesis of photoinitiator 2959 from the compound (CAS:159119-01-4) was as follows: a 25 mL Schlenk reaction tube was taken and N-bromosuccinimide (NBS) 18 mg (0.1 mmol) was added sequentially as catalyst, 4'-(2-hydroxyethoxy)-2-methylpropiophenone 105 mg (0.5 mmol), and dimethyl sulfoxide (DMSO) 1 mL as oxidizing reagent and solvent. ), and dimethyl sulfoxide (DMSO) 1 mL as oxidizer, carbonylation reagent and solvent. The reaction mixture was stirred at 100 °C for 24 hours. Upon completion of the reaction, 15 mL of ethyl acetate and 3 mL of brine were added to the reaction mixture for extraction, which was then extracted three times with ethyl acetate. All organic phases were combined and purified by column chromatographic separation to give a final purity of 103 mg of 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone in 92% yield.

159119-01-4
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106797-53-9
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Yield:106797-53-9 92%

Reaction Conditions:

with N-Bromosuccinimide;dimethyl sulfoxide at 60; for 24 h;Schlenk technique;

Steps:

26 Embodiment 262 - hydroxy -4 ' - (2 - hydroxy ethoxy group) -2 - methylpropiophenone preparation

Taking a 25 ml Schlenk reaction tube, adding N - bromo succimide (NBS) 18 mg (0.1mmol) as catalyst, 4' - (2 - hydroxy ethoxy group) -2 - methylpropiophenone 105 mg (0.5mmol), dimethyl sulfoxide (DMSO) 1 ml as the oxidizing agent, carbonylating and solvent, for 100 °C stirring for 24 hours. After the reaction by adding ethyl acetate 15 ml, salt water 3 ml, ethyl acetate 3 times, the combined organic phase, column chromatography separation to obtain 2 - hydroxy -4 ' - (2 - hydroxy ethoxy group) -2 - methylpropiophenone pure product 103 mg, yield 92%.

References:

CN104710256,2017,B Location in patent:Paragraph 0174-0177