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Sodium Thiosulfate → 4-Amino-3-fluoro-5-iodobenzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Thiosulfate | HCID 24477 | — |
| 反応物 | Iodine chloride | HCID 24640 | — |
| 反応物 | 4-Amino-3-fluorobenzonitrile | HCID 2756431 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Amino-3-fluoro-5-iodobenzonitrile | HCID 44203120 | — |
反応手順
A 25 ml of two-neck round bottom flask was filled with argon gas and the solution of 4-amino-3-fluoro-benzonitrile (300 mg, 2.204 mmol, 1 equiv.) in methylenechloride was put into the flask. To the solution was added iodomonochloride (393.6 mg, 2.424 mmol, 1.1 equiv.) and stirred for 1 hour. After confirming the completion of the reaction with TLC, to resulting solution was added saturated sodium thiosulphate solution and stirred. The reaction solution was extracted with methylenechloride, washed with water(twice) and brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The obtained liquid was column-chromatographed (n-hexane/ethylacetate=3/1) to yield a brown liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07960584B2 |
| 出典データセット | uspto-grants-2011_06 |
| ORD ID | ord-3323ce58260142188affe4053a67c887 |
| 出典メモ | uspto-grants-2011_06 |