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ChemicalBook CAS DataBase List Boron Standard Metal Solution
7697-32-7

Boron Standard Metal Solution synthesis

10synthesis methods
-

Yield: 98%

Reaction Conditions:

with potassium hydroxide in ethanol for 22 h;Reflux;

Steps:

1 Step 1 : Synthesis of 4-Brom o-3.5-dim ethyl benzoic acid (Int-5A)
4-Bromo-3,5-dimethylbenzonitrile (10 g, 48 mmol) was taken in ethanol (50 ml) and a solution of potassium hydroxide (13 g in 15 ml water) was added to it. The solution was heated to reflux for 22 hours. After cooling in an ice-bath, it was quenched by slowly adding 2.5 M sulfuric acid solution. The precipitated solids were collected by filtration and washed with water. After air-drying, the solids were taken up in toluene and solvent was removed to get dry powder. This was dried under vacuum to give the product as a light brown powder (10.7 g, 98%). 1H NMR (400 MHz, CHLOROF ORM-if) d ppm 7.82 (s, 2 H) 2.46 - 2.52 (m, 6 H).

References:

EPIODYNE, INC.;MEDINA, Julio Cesar;MCGEE, Larry;WEI, Zhi-Liang;SADLOWSKI, Corinne;SEIDL, Frederick;BHATT, Ulhas;WANG, Xiaodong;NGUYEN, Thomas;SPERANDIO, David;DING, Pingyu;NERURKAR, Alok;LI, Yihong;DUQUETTE, Jason WO2019/195634, 2019, A1 Location in patent:Page/Page column 223-224