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ChemicalBook CAS DataBase List ETHYL 2 5-DIHYDROXYBENZOATE 97

ETHYL 2 5-DIHYDROXYBENZOATE 97 synthesis

9synthesis methods
-

Yield:3943-91-7 99%

Reaction Conditions:

at 120; for 4 h;

Steps:

Representative procedure (compound 1)

General procedure: In a 50 mL two-necked round-bottomed flask equipped with a magnetic stirring bar, a reflux condenser and a calcium chloride drying tube was placed nicotinic acid (1 g, 8.1 mmol) suspended in boron trifluoride etherate (10 mL). The reaction mixture was stirred and heated to 120 °C overnight during which the creamy reaction mixture changed into a brownish solution. Thin layer chromatography (hexane/ethyl acetate 3:1) revealed complete reaction. The cooled reaction mixture was diluted with water (25 mL) and extracted with ethyl acetate (3 x 10 mL). The combined organic extract was washed to the end of effervescence with a saturated solution of NaHCO3. The organic phase was dried over anhydrous Na2SO4 and concentrated in vacuo giving a crude yield of 1.11 g (92%).

References:

Jumbam, Ndze D.;Maganga, Yamkela;Masamba, Wayiza;Mbunye, Nomthandazo I.;Mgoqi, Esethu;Mtwa, Sphumusa [Bulletin of the Chemical Society of Ethiopia,2018,vol. 32,# 2,p. 387 - 392]

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