4,7-dibroMo-5,6-dinitrobenzo[c][1,2,5]thiadiazole synthesis
- Product Name:4,7-dibroMo-5,6-dinitrobenzo[c][1,2,5]thiadiazole
- CAS Number:76186-72-6
- Molecular formula:C6Br2N4O4S
- Molecular Weight:383.96
15155-41-6
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Yield:76186-72-6 95%
Reaction Conditions:
with sulfuric acid;nitric acid in toluene at 20; for 20 h;
Steps:
A1-1 Synthesis (A1-1)
Synthesis (A1-1)Thus, compound (b) (4,7-dibromo-5,6-dinitro-benzo [1,2,5]thiadiazole) 60 g of HPLC purity 95% was obtained.[0168] in a 5-liter flask, Fuming nitric acid 1500ml was put& cooled. to this, keeping at 10 ~ 50 sulfuric acid 1500ml wassplit-added. Further to this, compound (a) 150gwhich is dibromo benzothiadiazole of raw material Was addedin small portions over a period of one hour. It was carried out so thatthe Solution temperature at that time was 5 or less.After the total amount of addition, it was allowed to react for 20 hours atroom temperature (25 ). Afterthe reaction, the reaction solution was poured into ice 3kg, and stirredovernight. Then filtered and washed with methanol, heptane. Then, the remainingafter filtration was allowed to heat-dissolved in toluene of 200ml, and afterslow cooling to room temperature, it was filtered and washed the remaining witha small amount of toluene and dried under reduced pressure.
References:
JP2016/6047,2016,A Location in patent:Paragraph 0165-0166;0167
22706-22-5
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76186-72-6
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