6-NITRO-2-PHENYLBENZOTHIAZOLE synthesis
- Product Name:6-NITRO-2-PHENYLBENZOTHIAZOLE
- CAS Number:38338-23-7
- Molecular formula:C13H8N2O2S
- Molecular Weight:256.28
Yield:38338-23-7 95.8%
Reaction Conditions:
with bis(benzonitrile)palladium(II) dichloride;1,10-Phenanthroline;1-aza-4,6,11-trioxa-5-boratricyclo[3.3.3.0(1,5)]undecane;diisopropylamine in water;dimethyl sulfoxide;butan-1-ol at 70; for 9 h;Reagent/catalyst;Solvent;
Steps:
4 Example 4
To a suitable amount of three-component solvent (dimethylsulfoxide (DMSO) in a volume ratio of 6: 1: 1, a mixture of H2O and n-butanol at room temperature) was added 100 mmol of the compound of the above formula Compound and 200 mmol of the compound of formula (II), 6 mmol of catalyst Pd (PhCN) 2 Cl2, 125 mmol of base diisopropanolamine and 17 mmol of accelerator (3.4 mmol of 1,10-phenanthroline and 13.6 mmol of triethanolamine boron Acid ester mixture); the temperature is raised to 70 ° C and the reaction is stirred at this temperature for 9 hours.After the reaction is completed, the reaction system is naturally cooled to room temperature, sufficient deionized water is added enough to wash 2-3 times, and then extracted with enough chloroform, thoroughly shaken, the upper organic phase is taken, dried over anhydrous sodium sulfate, filtered, The resulting residue was subjected to pressure distillation over 300-400 mesh silica gel column chromatography using a 2: 1 by volume mixture of acetone and ethyl acetate as the elution solvent to obtain the compound of formula (III) in a yield of 95.8 %
References:
CN105037294,2018,B Location in patent:Page/Page column 6-9
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