反应 #1715678
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08394772B2
反应条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a stirred solution of LAH (3.01 g, 79.10 mmol) in THF (80 ml) at 0° C. was added 2,2-dimethyl-4H-benzo[1,4]oxazin-3-one (7.00 g, 39.5 mmol) in portions and stirred the reaction mixture at 25° C. for 1 h and then 50° C. for 3 h. Reaction mixture was quenched by the addition cold saturated sodium sulfate solution and it was filtered through celite and extracted with DCM (100 ml×2), washed with brine (50 ml), dried over sodium sulfate, concentrated to give 2,2-dimethyl-3,4-dihydro-2H-benzo[1,4]oxazine (6.09 g), which was used as such for the next reaction without purification 50° C. for 3 h Reaction mixture was quenched by the addition cold saturated sodium sulfate solution and it was filtered through celite extracted with DCM (100 ml×2) washed with brine (50 ml) dried over sodium sulfate concentrated
来源 ID: ord-027ee0f367c64bb7bd47eb84e033b16e