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CAS No. : | 20776-63-0 | MDL No. : | MFCD03618451 |
Formula : | C7H5Cl2NO2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | VNOYJBSEORILIE-UHFFFAOYSA-N |
M.W : | 206.03 | Pubchem ID : | 290498 |
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 |
---|---|---|
82% | With sodium hydroxide; dihydrogen peroxide; In water; for 2h; | At room temperature, to a solution of the intermediate I-2 (5.0 g, 23.1 mmol) prepared by the above peparation example I(2) in 75 mL 1N NaOH (aq) was added portionwise hydrogen peroxide (28% v/v, 10 mL). The reaction mixture was filtered after stirring for 2 hours to remove insoluble dark brown solid. The filterate was then carefully acidified to pH 2 by conc. hydrochloric acid. The formed yellow precipitates were collected, washed with water, and dried in vacuo. The objective compound (3.90 g, 82%) was obtained as ivory-colored solid by recrystalization from benzene: TLC Rf=0.1 (EtOAc:n-hexane=1:1); m.p. 188-189 C.; 1H NMR (DMSO-d6) delta 6.76 (d, J=1.9 Hz, 1H, ArH), 6.85 (d, J=1.9 Hz, 1H, ArH); MS (EI) m/e 206 [M+], 162 [M+-CO2]. |
82% | 3) Intermediate I-3; 2-amino-4,6-dichloro benzoic acid; At room temperature, to a solution of the intermediate I-2 (5.0 g, 23.1 mmol) prepared by the above peparation example I(2) in 75 mL 1N NaOH (aq) was added portionwise hydrogen peroxide (28 % v/v, 10 mL). The reaction mixture was filtered after stirring for 2 hours to remove insoluble dark brown solid. The filterate was then carefully acidified to pH 2 by conc. hydrochloric acid. The formed yellow precipitates were collected, washed with water, and dried in vacuo. The objective compound (3.90 g, 82 %) was obtained as ivory-colored solid by recrystalization from benzene: TLC Rf = 0.1 (EtOAc:n-hexane = 1:1); m.p. 188 - 189 C; 1H NMR (DMSO-d6) delta 6.76 (d, J = 1. 9 Hz, 1H, ArH), 6.85 (d, J = 1. 9 Hz, 1H, ArH); MS(EI) m/e 206[M+], 162[M+-CO2]. | |
82% | Step 3: Preparation of 2-amino-4,6-dichlorobenzoic acidTo a solution of 4,6-dihloro-lH-indole-2,3-dione (5.0 g, 23.1 mmol) in 75 ml of 1 N <n="28"/>NaOH was partially added hydrogen peroxide (28 % v/v, 10 ml) at room temperature. After stirring the mixture for 2 hours, an insoluble dark brown solid was removed by filtration. The filtrate was acidified with a cone, hydrochloric acid to a pH of 2. The yellow precipitate thus formed was harvested, washed with distilled water, and dried in a vacuum. Recrystallization in benzene produced the title compound as an ivory solid (3.90 g, 82%).TLC Rf= 0.1 (ethylacetate : n-hexane = 1:1); m.p. 188 - 189 C;1HNMR (DMSO-de) delta 6.76 (d, IH5J= 1.9 Hz5 ArH), 6.85 (d, IH5J= 1.9 Hz5 ArH);MS(EI) m/e 206 [M+], 162 [M+-CO2]. |
82% | Step 3 Preparation of 2-amino-4,6-dichlorobenzoic acid To a solution of 4,6-dihloro-1H-indole-2,3-dione (5.0 g, 23.1 mmol) in 75 ml of 1 N NaOH was partially added hydrogen peroxide (28% v/v, 10 ml) at room temperature. After stirring the mixture for 2 hours, an insoluble dark brown solid was removed by filtration. The filtrate was acidified with a cone, hydrochloric acid to a pH of 2. The yellow precipitate thus formed was harvested, washed with distilled water, and dried in a vacuum. Recrystallization in benzene produced the title compound as an ivory solid (3.90 g, 82%). TLC Rf=0.1 (ethylacetate: n-hexane=1:1); m.p. 188-189 C.; 1H NMR (DMSO-d6) delta 6.76 (d, 1H, J=1.9 Hz, ArH), 6.85 (d, 1H, J=1.9 Hz, ArH); MS (EI) m/e 206 [M+], 162 [M+-CO2]. |
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