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Ammonium Acetate → N-(tert-Butyl)-2-amino-2-(4-fluorophenyl)ethanesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 反応物 | N-(tert-Butyl)-2-(4-fluorophenyl)-2-oxoethanesulfonamide | HCID 68288463 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N-(tert-Butyl)-2-amino-2-(4-fluorophenyl)ethanesulfonamide | HCID 68287917 | 105.7% |
反応手順
A solution of N-(tert-butyl)-2-(4-fluorophenyl)-2-oxoethanesulfonamide (657 mg), ammonium acetate (1.85 g) and sodium cyanoborohydride (166 mg) was stirred in methanol (12 ml) at 60° C. for 17 hours. The reaction solution was concentrated by rotary evaporation and the residue was taken up in ethyl acetate (50 ml). Then it was washed with 0.5 N aqueous sodium hydroxide solution (50 ml) and with saturated sodium chloride solution (50 ml), and the organic phase was dried over MgSO4, filtered and concentrated under reduced pressure. This gave the product (697 mg) with a molecular weight of 274.3 g/mol (C12H19FN2O2S), MS (ESI): m/e=275 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08828995B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-e6e383aa11d742978b08a562cc141a0b |
| 出典メモ | uspto-grants-2014_09 |