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N-Methyl-N-nitrosourea → Methyl 4-cyclopropyl-2,3,5,6-tetrafluorobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-Methyl-N-nitrosourea | HCID 12699 | — |
| 反応物 | Methyl 2,3,5,6-tetrafluoro-4-vinylbenzoate | HCID 15136253 | — |
| 反応物 | Diazomethane diethylether | HCID 21186548 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | Methyl 4-cyclopropyl-2,3,5,6-tetrafluorobenzoate | HCID 15136255 | 99.1% |
反応手順
In 10 ml of diethyl ether was dissolved 2.0 g of methyl 2,3,5,6-tetrafluoro-4-vinylbenzoate. To the resulting solution was added, with ice-cooling, a diazomethane-diethyl ether solution prepared from 3.0 g of N-methyl-N-nitrosourea. The resulting mixture was stirred at room temperature for 2 hours. The reaction mixture was concentrated under reduced pressure. The residue obtained was dissolved in 15 ml of xylene and the resulting solution was refluxed for 1 hour. The reaction mixture was concentrated under reduced pressure to obtain 2.1 g (yield: 99.1%) of methyl 4-cyclopropyl-2,3,5,6-tetrafluorobenzoate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04990508 |
| 出典データセット | uspto-grants-1991_02 |
| ORD ID | ord-b8ebed55f0cf475f9f7db15b818bd6ba |
| 出典メモ | uspto-grants-1991_02 |