Bispyribac-sodium synthesis
- Product Name:Bispyribac-sodium
- CAS Number:125401-92-5
- Molecular formula:C19H17N4NaO8
- Molecular Weight:452.35
303-07-1
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$10.00/5g
113583-35-0
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$6.00/10g
125401-92-5
230 suppliers
$25.00/25mg
Yield:125401-92-5 385 g
Reaction Conditions:
Stage #1:2,6-Dihydroxybenzoic acid with sodium hydride in dimethyl sulfoxide;mineral oil at 30 - 32; for 2 h;
Stage #2:4,6-dimethoxypyrimidin-2-yl methyl sulfone in dimethyl sulfoxide;mineral oil at 30 - 32;Concentration;Time;
Steps:
1 Preparation of Bispyribac sodium (Examples 1-5) Example-1
Preparation of Bispyribac sodium (Examples 1-5) Example-1 : A clear solution of 154 gm of 2,6-dihydroxy benzoic acid in 500 ml Dimethyl sulfoxide is added over 2-3 hr into a mixture of commercial available (60% emulsion in oil) 130 gm of Sodium hydride in 2 lit. of Dimethyl sulfoxide at 30-32°C . Mass is further stirred for 2 hr at 30-32°C and 480 gm of 4,6-Dimethoxy-2-(Methyl Sulfonyl)-pyrimidine is added into it over 2 hr. Reaction is maintained at 30-32°C till completion to get Bispyribac sodium. The reaction was monitored by HPLC. Mass is filtered, washed with DMSO. Wet solids were reslurried into 1000 ml of methanol & then in 1000 ml of 75% aq. Methanol. Wet solids were dried in oven to get 435 gm of Bispyribac sodium. This Bispyribac sodium is reslurried into 1200 ml of Toluene at reflux temperature, cooled, filtered & dried to give 385 gm of Bispyribac sodium ( purity 98.7% HPLC).
References:
GHARDA CHEMICALS LTD;MATHUR SUCHET S;VIJAYAN ANITH;NOUGARE VINAYAK H;BHOSALE SACHIN R;DAPAKE MANGESH K;PARKAR SURESHKUMAR D;DAMANIA PRAGNESH D;JAGTAP NANDKISHOR S;KALIRAJAN A;KHAMKAR RAHUL H;JAIN NANDKUMAR J;MORE MAHENDRA M;AHER SATYAWAN B;PADWAL SACHIN S WO2014/128719, 2014, A2 Location in patent:Page/Page column 13-14
125401-75-4
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125401-92-5
230 suppliers
$25.00/25mg
90905-46-7
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$15.00/5g
125401-92-5
230 suppliers
$25.00/25mg