反应 #3228636
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07259266B2
反应条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: The (2-amino-5-chloro-3-methylphenyl)methanol (10.8 g, 63.1 mmol) was dissolved in tetrahydrofuran (20 mL). Dichloromethane (50 mL) was added along with activated carbon (16.3 g). Activated manganese dioxide (16.8 g, 189 mmol) was added and the solution stirred at 40° C. for 16 h. The solution was cooled to room temperature and vacuum filtered through a celite. The solvent was removed at reduced pressure and the 2-amino-5-chloro-3-methylbenzaldehyde (7.90 g, 46.0 mmol) obtained by recrystallization from diethyl ether/hexanes (1:10, 100 mL). HRMS m/z 169.0280; calcd 169.0294. The solution was cooled to room temperature vacuum filtered through a celite The solvent was removed at reduced pressure
来源 ID: ord-c053bb4c251540a594a93e314bb11973