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CAS No. : | 21598-06-1 | MDL No. : | MFCD00005615 |
Formula : | C9H7NO3 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | BIMHWDJKNOMNLD-UHFFFAOYSA-N |
M.W : | 177.16 | Pubchem ID : | 88958 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | 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 |
---|---|---|
92% | With hydrogenchloride; for 4h;Reflux; Inert atmosphere; | 5-Hydroxyindole-2-carboxylicacid 30 (1.53 g, 8.6 mmol) was boiled under reflux in EtOH (100 mL)saturated with HCl under N2 for 4 h. The evaporation residue, EtOAc,was washed (water, brine). Drying, evaporation and chromatography (CH2Cl2? CH2Cl2 / EtOAc 4:1) gave 31 (1.64 g, 92%) as awhite solid: mp 152-154C (lit.3 146-148C); IR numax 3316,3209, 1696 cm-1; 1H NMR ((CD3)2SO) d 1.38 (3 H, t, J = 7.1 Hz, Me), 4.37 (2 H, q, J= 7.1 Hz, CH2), 6.86 (1 H, dd, J= 8.8, 2.4 Hz, 6-H), 6.97 (1 H, d, J= 2.3 Hz, 4-H), 7.00 (1 H, dd, J =2.1, 0.8 Hz, 3-H), 7.32 (1 H, d, J =8.8 Hz, 7-H), 8.93 (1 H, s, OH), 11.60 (1 H, s, NH). 13C NMR ((CD3)2SO)d 14.29 (Me), 60.17 (CH2), 104.43(4-C), 106.66 (3-C), 113.07 (7-C), 116.15 (6-C), 127.36 (2-C or 3a-C), 127.44 (3a-C or 2-C),132.21 (7a-C), 151.34 (5-C), 161.30 (C=O) |
86% | With sulfuric acid; for 12h;Reflux; | To the solution of compound 1 (5 g, 0.028 mol) in EtOH (250 mL) was added H2SO4(0.5 mL). The mixture was heated to reflux for 12 h. After cooled to RT, the reaction mixture was concentrated and dissolved in DCM (100 mL). The DCM layer was washed with sat.NaHCO3, dried over Na2SO4, concentrated to give compound 2 (5.0 g, 86% yield) as white solid. |