Chlorphenesin synthesis
- Product Name:Chlorphenesin
- CAS Number:104-29-0
- Molecular formula:C9H11ClO3
- Molecular Weight:202.63
Yield:104-29-0 95.1%
Reaction Conditions:
with tetrabutylammomium bromide;sodium hydroxide at 105; for 3 h;Concentration;Reagent/catalyst;
Steps:
5
Take 500ml three bottles, A mixture of 74.8 g (98.05%) of 3-chloro-1,2-propanediol (0.65 mol) P-chlorophenol 33.2 g (0.26 mol), Concentration of 10% NaOH solution 68.0g, Tetrabutylammonium bromide 1.28 g, The reaction system was heated to 105 ° C, Reaction for 1 h. 18.0 g (0.14 mol) of p-chlorophenol, 10% NaOH solution 96.8 g, 3-chloro-1,2-propanediol 9.2 g (content 98.05%) (0.08 mol) at this time, The molar ratio of p-chlorophenol to 3-chloro-1,2-propanediol was 1: 1.85, The molar ratio of p-chlorophenol to sodium hydroxide is 1: 1.85, The molar ratio of p-chlorophenol to tetrabutylammonium bromide was 1: 0.005, Continue to react 2h, Cooling to 20 , Add dilute hydrochloric acid to adjust the pH to 6.0. After standing for some time, Separate two phases, Take the lower organic phase, Gas chromatography monitoring, The conversion rate was 98.9% (see Figure 1) To the reaction solution was added 200 ml of water and 300 ml of trichloromethane, The volume ratio of chloroform to water is 3: 2, Into the ice water mixing, There are white solid precipitation, Stir, Suction filter. 40 vacuum drying, The product weighs 77.08g, the yield is 95.1%, the content is 99.64%.
References:
CN105016989,2017,B Location in patent:Paragraph 0082; 0083
556-52-5
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$17.67/1gm:
106-48-9
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104-29-0
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$8.00/10g
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104-29-0
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