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CAS No. : | 75319-02-7 | MDL No. : | MFCD03425682 |
Formula : | C8H9ClN2O | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 184.62 g/mol | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P264-P270-P271-P280-P301+P312+P330-P302+P352-P304+P340+P312-P305+P351+P338-P332+P313-P337+P313-P362-P403+P233-P405-P501 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
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* 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 |
---|---|---|
With sodium hydroxide In ethanol; water | 1 Preparation of 4-Chloro-2-methylbenzoic Acid, 2,2-bis(2-fluoroethyl)hydrazide (Compound No. 1) Example 1 Preparation of 4-Chloro-2-methylbenzoic Acid, 2,2-bis(2-fluoroethyl)hydrazide (Compound No. 1) To 50 mL of ethanol was added 5 gm of 4-chloro-2-methylbenzhydrazide followed by 4 gm of sodium hydroxide pellets. After stirring for 15 min, 7.5 gm of 1-bromo-2-fluoroethane was added dropwise. After this addition was complete, the resulting mixture was stirred for 4 hours, then diluted with 100 mL of water, and, finally, extracted with ethyl acetate. Upon evaporation of the solvent, an oil remained which was purified by chromatography, to produce 1.7 g of 4-chloro-2-methylbenzoic acid, 2,2-bis(2-fluoroethyl)hydrazide as an off white solid, mp 85°-87° C. The compounds summarized in Table 1 were prepared using an analogous procedure. Each of the compounds is characterized by its NMR data. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrazine hydrate In ethanol for 8h; Reflux; | ||
With hydrazine hydrate In methanol at 80℃; for 4h; | preparation of intermediate 2 General procedure: At the 250 cm3double-mouth bottle, 13.5 mmol of themethyl benzoate derivatives was added to 100 cm3of methanol,added 6.75 cm3of hydrazine hydrate (108 mmol) tothe reaction mixture slowly. After that warming to 80 °Cand reflux for 4 h until the reaction was completed, thenconcentrated under reducing pressure to remove methanol,filtering and drying to get white solid 2. |
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