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CAS No. : | 16152-51-5 | MDL No. : | MFCD01074614 |
Formula : | C9H13BO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | IAEUFBDMVKQCLU-UHFFFAOYSA-N |
M.W : | 164.01 | Pubchem ID : | 2773480 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | 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 |
---|---|---|
90% | With sodium carbonate;tetrakis(triphenylphosphine) palladium(0); In ethanol; water; toluene; at 110℃; for 3h; | An aqueous sodium carbonate solution (2M, 8.0 ml), ethanol (5.4 ml), 4-isopropylphenylboronic acid (1.6 g, 9.6 mmol) and tetrakis(triphenylphosphine)palladium (0.19 g, 0.16 mmol) were added to a solution of <strong>[621-38-5]3-bromoacetanilide</strong> (1.7 g, 8.0 mmol) obtained from 3-bromoaniline by the same process as in Reference Example 5 in toluene (20 ml), and the resulting mixture was heated to 110C. After 3 hours of stirring, a saturated aqueous sodium chloride solution was added thereto, followed by extraction with chloroform. The extract solution was washed with a saturated aqueous sodium chloride solution, dried over sodium sulfate and then concentrated under reduced pressure. The resulting residue was purified by the use of a silica gel column (chloroform : methanol = 50 : 1). Then, the purified residue was recrystallized from chloroform/hexane to obtain the desired compound (1.8 g, 90%). 1H-NMR (CDCl3) delta 1.28(d, J=7.0Hz, 6H), 1.58-1.59(m, 1H), 2.20(s, 3H), 2.95(tt, J=7.0, 7.0Hz, 1H), 7.26-7.40(m, 4H), 7.49-7.53(m, 3H), 7.69(br.s, 1H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
100% | With bis-triphenylphosphine-palladium(II) chloride; potassium phosphate; triphenylphosphine; In 1,2-dimethoxyethane; water; at 90℃; for 8h; | 38 g (180 mmol) of tripotassium phosphate, 100 mL of distilled water, 100 mL of DME, 11 g (67.1 mmol) of 4-isopropylphenylboronic acid, 11.0 g (56.4 mmol) of <strong>[16657-07-1]7-bromo-1H-indene</strong>, 323 mg (0.460 mmol) of dichlorobis(triphenylphosphine)palladium, and 432 mg (1.65 mmol) of triphenyl phosphine were put into a 500-mL glass reactor in that order, and then heated under reflux at 90 C. for 8 hours. This was left cooled to room temperature, then the reaction liquid was poured into 100 mL of distilled water, transferred into a separatory funnel, and extracted three times with hexane. At room temperature 5 mL of concentrated hydrochloric acid was added to the hexane solution, then stirred at room temperature for 30 minutes, the palladium compound was precipitated, filtered out through filter paper, and the filtrate was washed three times each with saturated saline water and distilled water, and dried with sodium sulfate. Sodium sulfate was filtered away, the solvent was evaporated away under reduced pressure, and the residue was purified through silica gel column chromatography (developing solvent, hexane/diisopropyl ether=20/1) to give 13.2 g (yield 100%) of 4-(4-isopropylphenyl)indene as a pale red oil. |
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