関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | p-Nitroacetophenone | HCID 7487 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | Dimethoxymethanamine | HCID 14871319 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-(4-Nitrophenyl)-1H-pyrazole | HCID 2737071 | 98% |
反応手順
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
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07419988B2 |
|---|
| 出典データセット | uspto-grants-2008_09 |
|---|
| ORD ID | ord-33f6c07783a5412baec25e75d0936082 |
|---|
| 出典メモ | uspto-grants-2008_09 |
|---|