反应 #90839
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07419988B2
反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 1-(4-nitrophenyl)ethanone (605.5 mmol) and bis(methyloxy)methanamine (726 mmol) in N,N-dimethylformamide (1000 mL) was stirred for 1 h at 80° C. The reaction was concentrated in vacuo, the residue was dissolved in ethanol (1000 mL) and treated with hydrazine monohydrate (1816 mmol). After the reaction stirred 2 h at 70° C. it was cooled to room temperature and poured into ice-water (2000 mL). Product precipitated out of solution, which was filtered, washed with water (4×500 mL) and dried to provide the title product as a yellow powder (98%). ESMS [M+H]+: 190.2 The reaction was concentrated in vacuo the residue was dissolved in ethanol (1000 mL) was cooled to room temperature Product precipitated out of solution, which was filtered washed with water (4×500 mL) dried
来源 ID: ord-33f6c07783a5412baec25e75d0936082