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CAS No. : | 3470-45-9 | MDL No. : | MFCD03411486 |
Formula : | C10H8O3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | SLLCLJRVOCBDTC-UHFFFAOYSA-N |
M.W : | 176.17 | Pubchem ID : | 22620801 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-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 |
---|---|---|
With hydrogenchloride; In acetic acid; at 120.0℃; for 16.0h; | l-oxo-2,3-dihydro-lH-inden-5-carbonitrile (1.0 g) was suspended in a solution of concentrated hydrochloric acid (10 ml) and acetic acid (20 ml), and stirred at 12 00C for 16 hours. After cooling, the reaction solution was concentrated under reduced pressure, tert-butyl methyl ether and water was added and then stirred. The organic layer was dried over anhydrous magnesium sulfate. After removing the solvent by distillation under reduced pressure, l-oxo-2,3-dihydro-lH-inden-5-carboxyic acid (0.7 g) was obtained. <n="141"/>1H-NMR (acetone-^) delta : 2.69-2.75 (3H, m), 3.23-3.25 (3H, m), 7.74(1H, d), 8.04 (IH, d), 8.19(IH, s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium permanganate; tetrabutylammomium bromide; In toluene; | the preparation is carried out as in Example 19 for 1-oxoindane-4-carboxylic acid but from 22.3 g of 3-(1-oxoindan-5-yl)acrylic acid, 560 ml of distilled water, 370 ml of toluene, 4.95 g of tetrabutylammonium bromide and 47.4 g of potassium permanganate. 14.4 g of 1-oxoindane-5-carboxylic acid are obtained in the form of a cream-coloured solid melting at 270 C. 3-(1-Oxoindan-5-yl)acrylic acid can be prepared in the following way: |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With oxalyl dichloride;N,N-dimethyl-formamide; In dichloromethane; at 20.0℃; for 2.0h; | Step 9-1 : Synthesis of N-[2-ethyl-4-(l,l,l,2,3,3,3-heptafluoropropan-2-yl)-6- methylphenyl]- 1 - xoindane-carboxamide (Compound No. L- 1 ).[0212] 1 -Oxoindane-5-carboxylic acid (3.0 g) was suspended in methylene chloride (30 ml), and oxalyl chloride (1.8 g) and a small amount of N,N-dimethylformamide (2 to 3 drops) were added thereto, and then stirred at room temperature for 2 hours. Thereafter, the solvent and oxalyl chloride were distilled off under reduced pressure. Pyridine (1.6 g) and 2-ethyl-4-(1,1, 1,2,3 ,3,3-heptafluoropropan-2-yl)-6-methylaniline (1.6 g) dissolved in methylene chloride (30 ml) were added to the residue, and the mixture was stirred at room temperature overnight. The reaction solution was concentrated under reduced pressure and the residue was purified by column chromatography to obtain N-[2-ethyl-4-( 1,1, 1,2,3 ,3,3 -heptafluoropropan-2-yl)-6- methyIphenyl]-l-oxoindane-5-carboxamide (2.4 g, yield 53%).[0213] 1H-NMR (CDCl3): see the Table below. [0214] |
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