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CAS No. : | 158465-13-5 | MDL No. : | MFCD10693482 |
Formula : | C7H4Cl2N2S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | SZOSKIQVUBIDGL-UHFFFAOYSA-N |
M.W : | 219.09 | Pubchem ID : | 43120177 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
81% | With bromine In chloroform at 0 - 60℃; for 10 h; | j00330j To a solution of compound B-28 (1.0 g, 3.7 mmol) in chloroform (20 mL) at 0 °C was added bromine (1.2 g, 7.4 mmol). The mixture was stirred at 60 °C for 10 hours, then cooled to room temperature and filtered to collect the solid. The solid was washed with acetone (4 x 5 mL), then added into water (45 mL). The mixture was stirred at 95 °C for 30 mm, then adjusted to pH 9 with sodium hydroxide (0.5 M). The solid was collected by filtration and dried in vacuo to give compound B-29 (0.68 g, 81percent yield) as a purple gray solid. ‘H-NMR (CDC13, 400 MHz): 7.43 (d, J=1.6 Hz, 1H), 7.15 (d, J1.6 Hz, 1H), 5.32 (bs, 2H). |
42% | With dioxane dibromide In 1,4-dioxane; chloroform at 0 - 80℃; for 23 h; Inert atmosphere | In the (3,5-dichlorophenyl) thiourea (5 00mg, 2.26mg)The chloroform solution (4.0 ml), andIn a nitrogen environment at 0 ° CBromo-1,4-dioxane was added fathoms complexCompound (5 61mg, 2.26mol),The 0 ° C was stirred for 1.0 hours at 80 ° C for 22 h.The reaction mixture was cooled, concentrated under reduced pressure and the residue thus obtained was washed with water, recrystallized from ethanol. The powder separated by filtration to obtain it, and the filtrate was concentrated under reduced pressure and the obtained residue was washed with ethanol, collected by filtration to filter powder. Merger of two kinds of powder, to obtain the title compound (209mg, 42percent). |
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