| 54% |
With lithium aluminium tetrahydride; In tetrahydrofuran; at 0℃;Inert atmosphere; |
Lithium aluminum (740 mg, 19.4 mmol) was suspended in 15 mL of tetrahydrofuran,Under nitrogen protection, keep at 0 .A solution of <strong>[1074-36-8]4-mercaptobenzoic acid</strong> (1.0 g, 6.48 mmol) in tetrahydrofuran (15 mL) was slowly added dropwise to the lithium aluminum hydride tetrahydrofuran system, and the mixture was kept overnight.After quenching the reaction with 0.5 mL of water, the pH was adjusted to 2 with 2M hydrochloric acid, and extraction was performed with ethyl acetate.The organic phase was washed with water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure.Purification on a silica gel column gave 4-mercaptobenzyl alcohol (440 mg, 54%). |
| 54% |
With lithium aluminium tetrahydride; In tetrahydrofuran; at 0℃;Inert atmosphere; |
Lithium aluminum hydride (1.5 g, 38.8 mmol) was suspended in 30 mL of tetrahydrofuran, and the temperature was maintained at 0 C under the protection of nitrogen.A solution of <strong>[1074-36-8]4-mercaptobenzoic acid</strong> (2.0 g, 12.96 mmol) in tetrahydrofuran (20 mL) was slowly added dropwise to the lithium aluminum hydride tetrahydrofuran system, and the mixture was kept overnight.The reaction was quenched with 1.0 mL of water, the pH was adjusted to about 2 with 2M hydrochloric acid, and extracted with ethyl acetate.The organic phase was washed with water, saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure.Purification by silica gel column chromatography gave 4-mercaptobenzyl alcohol (880 mg, 54%). |
| 44% |
With lithium aluminium tetrahydride; In tetrahydrofuran; for 96h;Cooling with ice; Inert atmosphere; |
After LiAlH4 (5.51 g, 145 mmol) was added to dry tetrahydrofuran (THF, 170 mL), the mixture was stirred slightly under ice-cooling, and the inside of the reaction vessel was replaced with argon.Thereafter, a THF solution (130 mL) of <strong>[1074-36-8]4-mercaptobenzoic acid</strong> (7.57 g, 49.1 mmol) was added, and the mixture was stirred for 4 days.The reaction was stopped by adding a saturated aqueous solution of ammonium chloride, methanol was added, and then ultrasonic vibration was applied to dissolve the rattan oily substance, which was then dissolved with celite.After concentration under reduced pressure, ethyl acetate was added, and the mixture was washed twice with water and once with a saturated aqueous solution of sodium chloride.Collect the organic phase, dry over anhydrous sodium sulfate and filter the solution.After being obtained, it was concentrated under reduced pressure.Silica gel chromatography of the residue (hexane: acetic acid(Developed with chill = 1: 1, eluted with chloroform: methanol = 100: 0))There was obtained (4-mercaptophenyl) methanol (3.05 g, 21.8 mmol, yield 44%) as a white solid. |
|
With lithium aluminium tetrahydride; In tetrahydrofuran; at 0 - 20℃; for 16h; |
<strong>[1074-36-8]4-mercaptobenzoic acid</strong> (10.0 g, 64.9 mmol) was added to a solution of lithium aluminum hydride (3.69 g, 97.3 mmol) in THF (500 ml) at 0 C. The mixture was then warmed to room temperature and stirred for 16 h, then quenched with 2M HC1 to pH = 2. The aqueous solution was extracted with diethyl ether (3 x 500 mL), the combined organic layers dried with sodium sulfate, and the solvent removed in vacuo to give 8A, which was used without further purification (6.70 g, 43% purity, 20.6 mmol, 31% yield). |
|
With lithium aluminium tetrahydride; In tetrahydrofuran; at 0 - 20℃; for 16h; |
<strong>[1074-36-8]4-mercaptobenzoic acid</strong> (10.0 g, 64.9 mmol) was added to a solution of lithium aluminum hydride (3.69 g, 97.3 mmol) in THF (500 ml) at 0 C. The mixture was then warmed to room temperature and stirred for 16 h, then quenched with 2M HC1 to pH = 2. The aqueous solution was extracted with diethyl ether (3 x 500 mL), the combined organic layers dried with sodium sulfate, and the solvent removed in vacuo to give 17D, which was used without further purification (6.70 g, 43% purity, 20.6 mmol, 31% yield). |
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