To an ice-cooled solution of AlCl3(4.2 g; 31.5 mmol) in dry THF (25 mL) was added LiAlH4(0.5 g; 13.2 mmol) gradually,
and the resulting solution was stirred 10 min at room temperature and was subsequently refluxed during 30 min.
A solution of the SM in THF (25 mL) was added drop wise to the AlH2Cl solution, and after the addition was complete, reflux was maintained during 4 h: the reaction was monitoredby TLC. The reaction mixture was cooled with an icebath, and water was carefully added. The reaction product was extracted with CH2Cl2, and the combined extract was washed with 5percent H2SO4and water, dried with Drierite,and evaporated to dryness. The crude residue, which consisted essentially of a single spot on TLC was chromatographed on a column of silica gel (50 g). Elution with EtOAc–hexane (1 : 1, v/v) gave the TM which was recrystallized from EtOAc–hexane as colorless needles: mp 179–180°C; yield, 510 mg (64percent).
请参考,
不需要氯化铝
To an ice-cooled solution of AlCl3(4.2 g; 31.5 mmol) in dry THF (25 mL) was added LiAlH4(0.5 g; 13.2 mmol) gradually,
and the resulting solution was stirred 10 min at room temperature and was subsequently refluxed during 30 min.
A solution of the SM in THF (25 mL) was added drop wise to the AlH2Cl solution, and after the addition was complete, reflux was maintained during 4 h: the reaction was monitoredby TLC. The reaction mixture was cooled with an icebath, and water was carefully added. The reaction product was extracted with CH2Cl2, and the combined extract was washed with 5percent H2SO4and water, dried with Drierite,and evaporated to dryness. The crude residue, which consisted essentially of a single spot on TLC was chromatographed on a column of silica gel (50 g). Elution with EtOAc–hexane (1 : 1, v/v) gave the TM which was recrystallized from EtOAc–hexane as colorless needles: mp 179–180°C; yield, 510 mg (64percent).
请参考,
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可以把溶剂加点氢化铝锂处水!