酰酰还原制备酰

tal) was then added to the solution. Sodium hydroxide (5N, 230 mL) was then added to the mixture, which was then heated to reflux for about 30 minutes. After partitioning the aqueous and organic layers, the organic layer was collected. The aqueous layer was then extracted with tetrahydrofuran. The organic layers were combined and the solvents were then removed by evaporation. The resulting liquid was then partitioned between ethyl acetate and brine and was washed a second time with brine. The solution was

then dried over sodium sulfate and the solvents were removed in vacuo to yield 46.68 g of the desired product.

3 、NaBH4-Lewis acid 政治体制转变成苯甲酸

3.1 、NaBH4-BF3 政治体制转变成苯甲酸

To a solution of 8.8 g (39.8 mmol) of the starting material in 100 mL of dry THF, 4.52 g (119 mmol) of sodium borohydride was slowly added with cooling by ice under nitrogen atmosphere. To the obtained suspension, a solution of 16.1 mL of BF3-ether complex in 50ml of THF was slowly added with cooling by ice and then stirred for 4 hours with cooling by ice and for 4 hours at room temperature. Then, the reaction solution was poured into water, acidified by the addition of dilute hydrochloric acid and stirred for two hours. The solution was alkalized by the addition of an aqueous potassium hydroxide solution and extracted with ethyl acetate. The extract was dried on magnesium sulfate and filtered. The filtrate was concentrated and subjected to purification by silica gel column chromatography to give 2.2 g of the desired product.

3.2、 NaBH4-AlCl3 政治体制转变成苯甲酸

To a solution of the starting material (21.6 g, 58.6 mmol) and dimethoxyethane (175 mL) one adds portionwise at 15°C~20°C anhydrous aluminium chloride (31.3 g, 0.234 mol) and allows to stir further for 30min. One then adds NaBH4 (8.85 g, 0.234 mol) portionwise at15°C~20°C within 1/2 hr. After 3 hrs, stirring while cooling, ice-water (130mL) are carefully added dropwise, whereby the internal temperature is not to exceed 25°C. While cooling withice, one brings the PH value to 8.5 by addition of conc. NaOH, adds 75 mL ethyl acetate and filters. The precipitate is after-washed with ethyl acetate. After separation of the phases, the aqueous phase is also extracted with ethyl acetate, the organic extracts is dried, evaporated and combined with precipitate to afford the desired product.

4 、DIBAL 转变成苯甲酸【 会用转变成剂---DIBAL 】

A solution of the material (250 mg, 0.80 mmol) in dichloromethane (10 mL) was cooled to 0°C, then DIBAL-H (7.4 mL, 7.4 mmol of 1M in toluene) was added dropwise into the solution over 45 min. The mixture was stirred for 1 hour, then warmed to room temperature and stirred for 14 h. The reaction was quenched with potassium sodium tartrate aqueous solution. The mixture was extracted with dichloromethane (3×10 mL). The combined extracts were washed with water and brine, dried over sodium sulfate and concentrated under vacuum to afford an oil. Purification by column chromatography (silica; 90: 10, v/v, dichloromethane/methan- ol followed by 89: 10: 1 dichloromethane/methanol/ammonium hydroxide) produced the desired product (54 mg, 23% un-optimized yield) as a clear colorless oil.

5、 伯甲基经氧苯甲酸转变成后单甲福化范例【 会用转变成剂---氮化铝锂 】

600 mg (1.96 mmol) of the material in THF is slowly added dropwise to a suspension of 250 mg (6.59 mmol) of lithium aluminium hydride in 10 mL tetrahydrofuran. The reaction is stirred overnight and heated to 50.deg. C. for a further hour. Working up is carried out by the successive addition of 0.25 mL water, 0.25 mL 15percent NaOH solution and 0.75 mL water. After filtration the organic phase is dried over magnesium sulphate and the solvent is eliminated using the rotary evaporator. 350 mg of the product was obtained (81.1% yield).

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