Sodium gualenate synthesis
- Product Name:Sodium gualenate
- CAS Number:6223-35-4
- Molecular formula:C15H17NaO3S
- Molecular Weight:300.35
489-84-9
6223-35-4
(1) Preparation of sodium 3,8-dimethyl-5-isopropylchrysanthemum-1-sulfonate Under ice bath conditions, 4 mmol of guaiacol and 2 mL of acetic anhydride (Ac2O) were added to a 25 mL pear-shaped flask. Subsequently, a mixture of 1 mL of concentrated sulfuric acid (H2SO4) and 2 mL of acetic anhydride (Ac2O) was slowly added dropwise through a constant-pressure dropping funnel (with a drying tube fitted at the top). After the dropwise addition, the reaction mixture was stirred at room temperature for about 2 hours, during which the progress of the reaction was monitored by thin layer chromatography (TLC) until the feedstock completely disappeared. Upon completion of the reaction, the mixture solution was poured into 4 mL of water and the pH was adjusted to 8-9 by dropwise addition of sodium hydroxide (NaOH) solution.Subsequently, the mixture solution was cooled to promote the formation of a precipitate, filtration was carried out, and the precipitate was washed sequentially with cold water and petroleum ether, and was dried to give 1.05 g of a blue solid product. The yield was 87.5% and the melting point was 106-107 °C.
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6223-35-4
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Yield:6223-35-4 87.5%
Reaction Conditions:
with sulfuric acid;acetic anhydride at 20; for 2 h;Cooling with ice;
Steps:
14.1 (1)
Preparation of 3,8-dimethyl-5-isopropyl azulene-1-sodium sulphonate
(1)
Preparation of 3,8-dimethyl-5-isopropyl azulene-1-sodium sulphonate
Under ice bath, 25 ml pear-shaped flask was sequentially added with 4 mmol of guaiazulene, 2 ml of Ac2O, and then added with a mixture of 1 ml of concentrated H2SO4 and 2 ml of Ac2O through constant pressure dropping funnel (with a drying tube on the top).
After completion of dropwise addition, the mixture was stirred at room temperature for about 2 h and the reaction was tracked with TLC until the raw material disappears.
The mixture solution was poured into 4 ml of water, and then dropwise added with NaOH solution to adjust pH to 8-9.
Then the mixture solution was cooled to precipitate, leached, and washed with cold water and petroleum ether sequentially, dried, to obtain 1.05 g of blue solid. Yield: 87.5%. m.p. 106-107° C.
References:
Sichuan Guokang Pharmaceutical Co., Ltd;Zhang, Luyun;Yang, Fang;Shi, Wanqi;Zhang, Ping;Li, Ying;Yin, Shufan US2014/206741, 2014, A1 Location in patent:Paragraph 0108-0110
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6223-35-4
219 suppliers
$9.00/250mg