| 97% |
With water; potassium carbonate at 150℃; for 0.25h; Microwave irradiation; |
|
| 93% |
With cesium hydroxide; water; dimethyl sulfoxide at 60℃; for 12h; Schlenk technique; Green chemistry; |
|
| 91% |
With water at 130℃; for 1h; Microwave irradiation; |
|
| 89% |
With sodium hydroxide; poly(ethylene glycol)-400 for 0.0166667h; microwave irradiation; |
|
| 87% |
With Wilkinson's catalyst; Acetaldehyde oxime In toluene at 110℃; |
|
| 87% |
With Wilkinson's catalyst; Acetaldehyde oxime In toluene at 110℃; for 4h; |
|
| 84% |
With water; sodium hydroxide In ethanol at 90℃; for 17h; |
|
| 83% |
With Acetaldehyde oxime; [(eta.(5)-pentamethylcyclopentadienyl)Rh(H2O)3](OTf)2 In water at 80℃; for 12h; Schlenk technique; |
11 Example 11: 4-Acetylbenzamide
4-Acetylbenzonitrile (145 mg, 1 mmol), [Cp * Rh (H,2O)3] [OTf]2(3.0 mg, 0.005 mmol, 0.5 mol%), acetaldehyde oxime (65 mg, 1.1 mmol) and water (1 ml) were successively added to a 25 ml Schlenk reaction flask.The reaction mixture was allowed to react at 80 ° C for 12 hours, then cooled to room temperature, water was removed by rotary evaporation, and the column was separated to obtain the desired product, yield: 83% |
| 82% |
With [Ru(η6-C6Me6)Cl2(tris(dimethylamino)phosphine)]; water at 100℃; for 1.5h; Inert atmosphere; Sealed tube; |
|
| 80% |
With RuCl2(η6-C6Me6)(1-benzyl-3,5-diaza-1-azonia-7-phosphaadamantane chloride); water at 100℃; for 3h; Inert atmosphere; Neutral aq. solution; chemoselective reaction; |
|
| 80% |
With [RuCl2(η3:η3-C10H16){PMe2(OH)}]; water at 60℃; for 1h; Inert atmosphere; Schlenk technique; Sealed tube; |
|
| 80% |
With [RuCl2(η6-p-cymene)(P(4-C6H4F)2Cl)]; water at 40℃; for 3.5h; Sealed tube; Inert atmosphere; |
|
| 80% |
With [RuCl2(η3:η3-2,7-dimethylocta-2,6-diene-1,8-diyl)(PMe2OH)] In water at 60℃; for 1h; Inert atmosphere; Sealed tube; |
|
| 79% |
With water at 130℃; for 1h; Microwave irradiation; |
|
| 73% |
With [OsCl2(η6-p-cymene)(PMe2OH)]; water at 80℃; for 1h; Inert atmosphere; Sealed tube; |
|
| 73% |
With water In dimethyl sulfoxide at 100℃; Green chemistry; chemoselective reaction; |
|
| 73% |
With cis-[Mn(2,6-bis(di-tert-butylphosphinomethyl)pyridine)(CO)2]; water In <i>tert</i>-butyl alcohol at 90℃; for 24h; Green chemistry; |
|
| 68% |
With water extract of pomelo, peel at 150℃; for 0.75h; Sealed tube; Green chemistry; |
3.3. General Procedure for the Hydrolysis of Nitriles in WEPPA (Taking 1a as an Example
General procedure: Benzonitrile 1a (103 mg, 1.0 mmol) and WEPPA (2.0 mL) were added into a 10-mL closed tubewith a stir bar. Then the reaction was stirred in a closed vessel synthesis reactor at 150 C for 0.5 h.After cooling to ambient temperature, the resulting precipitate was collected by filtration, washed withice water, and further dried in a vacuum drying oven. The filtrate was evaporated under reducedpressure. The resultant residue was purified by silica gel column chromatography (eluent: petroleumether (35-60 C)/EtOAc = 2:1 to 0:1, v/v). Finally, these two parts were combined to produce the desiredbenzamide 2a with a 94% yield. |
| 45% |
With manganese(IV) oxide; silica gel for 0.233333h; microwave irradiation; |
|
| 40% |
With manganese(IV) oxide; silica gel In chlorobenzene for 5h; Heating; |
|
|
With water at 139.85℃; for 6h; |
|
|
With water for 6h; |
|
|
With nitrile hydratase from Rhodopseudomonas palustris CGA009 In methanol at 30℃; for 17h; aq. phosphate buffer; chemoselective reaction; |
|
| 97 %Chromat. |
With water at 80℃; for 6h; chemoselective reaction; |
|
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