4-Chloro-3-nitrobenzenesulfonyl chloride synthesis
- Product Name:4-Chloro-3-nitrobenzenesulfonyl chloride
- CAS Number:97-08-5
- Molecular formula:C6H3Cl2NO4S
- Molecular Weight:256.06
6671-49-4
97-08-5
Synthesis Example 2-2 Synthesis of 4-chloro-3-nitrobenzenesulfonyl chloride: to a reaction vial containing a mixture of 1280 g of potassium 4-chloro-3-nitrobenzenesulfonate, 1150 mL of acetonitrile, 250 mL of sulfoxide, and 30 mL of dimethylacetamide, 1240 mL of phosphinic acid chloride was added dropwise at a slow rate, while controlling the temperature within the reaction system to maintain a temperature of 60°C to 70°C. After the dropwise addition was completed, the reaction mixture was stirred at 73°C for 3 hours. Upon completion of the reaction, the reaction mixture was cooled with water, followed by the slow addition of 400 mL of water. The reaction mixture was poured into 5 L of ice water and the precipitated crystals were separated by filtration, washed with water and dried to give 1060 g of the target product 4-chloro-3-nitrobenzenesulfonyl chloride in 84% yield. The melting point of the product was 55 °C to 56 °C.
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Yield:97-08-5 71%
Reaction Conditions:
with sulfuric acid;nitric acid at 30 - 60;
Steps:
2
1L three bottles were added 500mL concentrated H2SO4, p-chlorobenzenesulfonyl chloride 190g (0.9mol, 1eq) and heated to 30 ° C, dropping fuming nitric acid 56. 7g (0. 9mo 1,1 eq) to keep the temperature below 60 ° C, After the addition the internal temperature was stirred overnight at 55 ° C, TLC (PE / EA = 10/1). The reaction was cooled, poured into ice water, extracted with DCM, dried, filtered and concentrated to give 3-nitro-4-chlorobenzenesulfonyl chloride, white crystals 163g, yield 71%
References:
Shaoyuan Science And Technology (Shanghai) Co., Ltd.;Mei Kai;Lu Yabing;Wu Yong CN106699614, 2017, A Location in patent:Paragraph 0020
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