Preparation method of 2-hydroxy-1-[4-(2-hydroxyethoxy) phenyl]-2-methyl-1-acetone
A hydroxyethoxy and phenyl technology, applied in the field of photoinitiator preparation, can solve the problems of catalyst loss, increased catalyst usage, loss of protective agent acetic acid, etc., and achieves the effect of high yield and purity
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Embodiment 1
[0078] This embodiment provides a preparation method of 2-hydroxy-1-[4-(2-hydroxyethoxy)phenyl]-2-methyl-1-propanone, which specifically includes the following steps:
[0079] (1) Add 94g of phenol, 84g of potassium hydroxide, 2g of PEG200 and 500g of dichloroethane in a four-neck flask to mix, heat up and reflux for dehydration reaction, GC monitors the conversion rate of phenol in the reaction solution > 98%, and then washes to neutral , reclaim ethylene dichloride by precipitation, and distill under reduced pressure to obtain the compound of formula b;
[0080]
[0081] The composition of the obtained compound of formula b was tested, and its liquid phase content was 98%, and the yield of the calculation step (1) was 94%;
[0082] The data result that the product obtained in step (1) is carried out to H-NMR analysis is as follows;
[0083] 1 H-NMR (CDCl3, 400Hz): 7.18-7.07 (m, 2H), 6.85-6.70 (m, 3H), 4.22 (t, 2H), 3.82 (t, 2H).
[0084] (2) Add the compound of formula...
Embodiment 2
[0097] The difference between this embodiment and Example 1 is only that in step (3), the equimolar amount of NaI is replaced by KI, and the equimolar amount and equal concentration of potassium hydroxide solution are replaced by sodium hydroxide solution. Other parameters and conditions and implementation Exactly the same as in Example 1.
[0098] The yield of photoinitiator 2959 in the step (3) of this embodiment is 85.7%, and the purity is 99.3%.
Embodiment 3
[0100] The difference between this embodiment and embodiment 1 is only that tetrabutylammonium bromide equimolar amount is replaced by tetrabutylammonium bisulfate, and other parameters and conditions are exactly the same as in embodiment 1.
[0101] The yield of photoinitiator 2959 in the step (3) of this embodiment is 83.0%, and the purity is 99.0%.
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