New learning discoveries about 4442-54-0

4442-54-0, As the paragraph descriping shows that 4442-54-0 is playing an increasingly important role.

4442-54-0, 2,3-Dihydro-1,4-benzodioxine-6-carboxylic acid is a benzodioxans compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5.0mmol of acetophenone and 5lmmol benzaldehyde into the 50ml round bottom burning, adding 20ml of anhydrous ethanol, magnetic stirring lOmin to mix evenly, slowly dropping 40percent NaOH solution 10ml, magnetic stirring, room temperature reaction 2h TLC). The product was precipitated as a solid, filtered and washed with a large amount of distilled water. The solid was washed three times with cold ethanol (3 ml each) and dried. The product was mixed with ethanol and acetone (volume ratio: Acetone = 10: 1). The compound obtained above was added to a 50 ml flask and heated to 80 ¡ã C in 20 ml of isopropanol (or 20 ml of ethanol). To the solution was added dropwise 2 mmol of hydrazine hydrate 80, The reaction was stirred at 80 ¡ã C for 5 h (TLC). After the end of the reaction, the distillation was carried out under reduced pressure until all of the ethanol was distilled off. The product was precipitated in a large amount as a solid, filtered and washed three times with cold ethanol (each about 3 ml). Within 20 min, 1.0 mmol of the obtained product, 1,4-benzodioxan-6-carboxylic acid was dissolved in 20 ml of methylene chloride at room temperature. 1.5 mmol of EDCI and 0.05 mmol of HOBt were added and the reaction was stirred for 10 h (TLC). After the completion of the reaction, the reaction solution was washed three times with 50 ml of water (150 ml each), and the resulting aqueous phase was combined three times, and extracted twice with 210 ml of ethyl acetate (70 ml each). The organic phase (dichloromethane and ethyl acetate) And distilled to dryness under reduced pressure to give a solid product which was recrystallized from a mixture of ethanol and acetone (volume ratio of ethanol: acetone = 10: 1) to give the title compound (white crystals).

4442-54-0, As the paragraph descriping shows that 4442-54-0 is playing an increasingly important role.

Reference£º
Patent; Nanjing University; Zhu, Hai Liang; Yang, yushun; Ding, Shu Ting; Zhang, Fei; Zhang, Yan Bin; Wang, Xiao Liang; Tang, Jian Feng; (22 pag.)CN103304546; (2016); B;,
Benzodioxan
1,4-Benzodioxane | C8H8O2 – PubChem