Bromfenac sodium synthesis
- Product Name:Bromfenac sodium
- CAS Number:91714-93-1
- Molecular formula:C15H11BrNNaO3
- Molecular Weight:356.15
91713-91-6
128 suppliers
$149.00/1g
91714-93-1
182 suppliers
$34.00/10mg
Yield:91714-93-1 83%
Reaction Conditions:
with sodium hydroxide in water at 100; for 1 h;
Steps:
1 Preparation of compound of formula 4
63 g of the compound of formula 3 and 2001 g of aqueous sodium hydroxide (concentration:4.0% aqueous sodium hydroxide solution,Configuration method: slowly add 81g of sodium hydroxide to 1920ml of purified water and mix well)Add to a three-port reaction bottle containing 1920mL,The mixture was heated to 100 ° C with stirring and reacted for 1 h.After completion of the reaction, the system was cooled to room temperature, suction filtered, and the filtrate was collected.Add the filtrate to a three-neck reaction flask and stir.Add 124 g of sodium chloride.After the addition, a large amount of solid was precipitated, stirring was continued for 1 h, and suction filtration was performed.The obtained solid was washed with 214 g of saturated brine and 300 mL of acetone, and then transferred to a three-neck reaction flask, and 63 mL of purified water was added thereto, and the mixture was heated to 81 ° C, and 630 mL of acetone was added dropwise. After the drop, the system is cooled to room temperature.Filter by suction, use 200 mL of purified water first:The acetone was washed 1:10 and then washed with 300 mL of acetone.The resulting solid was added to a three-neck reaction flask.Add 60 mL of purified water,Stir and heat to 70 ° C,After the system is dissolved,Add acetone 120mL,filter,The resulting filtrate was transferred to a three-neck reaction flask.Add 480 mL of acetone under stirring.Filtering,The solid was washed with 300 mL of acetone.Obtained 63.3g of yellow solid.The purity is 99.95%,Except for the relative retention time of 2.16, the impurity was 0.05%, and other impurities were not detected, and the yield was 83%.
References:
Yangzijiang Pharmaceutical Group Co., Ltd.;Wu Chuan;Cai Wei;Xu Haoyu;Han Dong;Zhou Weihai;Yuan Xinxiang;Liu Haifeng;Huang Shuping;Hao Xiubin CN108569975, 2018, A Location in patent:Paragraph 0034; 0039; 0040
91714-50-0
100 suppliers
$273.00/250mg
91714-93-1
182 suppliers
$34.00/10mg
1140-17-6
129 suppliers
$12.00/1g
91714-93-1
182 suppliers
$34.00/10mg
121-62-0
42 suppliers
$135.00/1g
91714-93-1
182 suppliers
$34.00/10mg
578-54-1
253 suppliers
$10.00/5g
91714-93-1
182 suppliers
$34.00/10mg