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Diazomethane → 5-Bromo-1-diazo-3-(3,4-dichlorophenyl)-2-pentanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diazomethane | HCID 9550 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1-Methyl-2-nitro-1-nitrosoguanidine | HCID 9562060 | — |
| 反応物 | alpha-(2-Bromoethyl)-3,4-dichlorophenylacetic acid chloride | HCID 54519315 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 5-Bromo-1-diazo-3-(3,4-dichlorophenyl)-2-pentanone | HCID 53781276 | — |
反応手順
Prepare a solution of diazomethane from 15 g of MNNG by reaction with 45 ml of 40% aqueous KOH topped with 150 ml. of Et2O and cool in an ice bath. Add an Et2O solution (40 ml.) of the product of Step 3 (8.2 g, 5 24.8 mmoles) in small volumes, stir the solution in the ice bath for 15 min, then heat to reflux for 30 min. Remove the solvent in vacuo. Purify the resulting mixture by flash chromatography on silica gel using CH2Cl2 as eluent. Yield: 7.0 g (IR: 2100 cm-1, 1630 cm-1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05840725 |
| 出典データセット | uspto-grants-1998_11 |
| ORD ID | ord-de8b5c7df0224edabc56be3a57f66237 |
| 出典メモ | uspto-grants-1998_11 |