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CAS No. : | 27328-68-3 | MDL No. : | MFCD09835467 |
Formula : | C9H7ClN2O2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | OIQMRQZOCUNAIN-UHFFFAOYSA-N |
M.W : | 210.62 | Pubchem ID : | 12470261 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
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 |
---|---|---|
Stage 2 (5-Chloro-1H-indazol-3-yl)acetic acid The amino acid obtained in Stage 1 is dissolved with 3 equivalents of sodium hydroxide pellets in 600 ml of water in a three-necked flask equipped with a thermometer, a mechanical stirrer, a dropping funnel and a reflux condenser surmounted by a bubbler. The mixture is brought to 30-40 C. and 5.7 g of active charcoal are added. Hydrazine monohydrate is slowly added (2.1 eq, i.e. 22.7 g). The mixture is stirred for 15 minutes at 30-40 C. and then for 3 hours at 80-85 C. The reaction mixture is cooled. After filtration, the reaction mixture is acidified with 75 ml of 36% hydrochloric acid. The precipitate formed is filtered off on sintered glass and then dried in a desiccator. Melting point: 193 C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In sodium hydroxide; water; | EXAMPLE 1 1-[(benzothiazol-2-yl)methyl]-1H-indazole-3-acetic acid To a vigorously stirring solution of 1H-indazole-3-acetic acid (0.88 g) in water (100 ml) containing sodium hydroxide (0.60 g) was added 2-(bromomethyl)benzothiazole (1.25 g) and the resulting mixture heated at 80 C. for 2.5 hours. The reaction solution was cooled to room temperature and extracted with ether (2*25 ml). The aqueous layer was collected and acidified to a pH of about 4.0 with concentrated HCl, and then extracted with ethyl acetate (2*20 ml). The organic layers were combined, dried and evaporated to a yellow solid (yield: 0.67 g), which was crystallized from benzene (m.p. 164-165 C.). Substituting a molar equivalent of <strong>[27328-68-3]5-chloro-1H-indazole-3-acetic acid</strong> for 1H-indazole-3-acetic acid, the same method was employed to prepare: 1-(benzothiazol-2-yl)methyl-<strong>[27328-68-3]5-chloro-1H-indazole-3-acetic acid</strong> (m.p. 213 C.). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogenchloride; sodium sulfite; sodium nitrite; In water; | EXAMPLE 1 Preparation of 5-chloro-1H-indazole-3-acetic acid: To a suspension of 2 -amino-5-chlorocinnamic acid (3.0 g) in water (35 ml), there is added conc. hydrochloric acid (11 ml). To the resulting solution cooled with ice, a solution of sodium nitrite (1.0 g) in water (2 ml) is dropwise added while stirring, and stirring is continued for 30 minutes. Anhydrous sodium sulfite (5.0 g) is portionwise added thereto. After stirring at room temperature for 1 hour, the resulting mixture is admixed with water (100 ml) and heated on an oil bath for 0.5 to 1 hour while refluxing. The reaction mixture is filtered. The collected material is washed with hot water. The washing water is combined with the filtrate and concentrated. The residue is crystallized from hot water to give 5-chloro-1H-indazole-3-acetic acid (0.7 g) as white needles melting at 205 C (decomp.) |
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