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4-Amino-3-nitrophenyl thiocyanate → 4-(Benzylthio)-2-nitroaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Amino-3-nitrophenyl thiocyanate | HCID 104677 | — |
| 反応物 | Benzyl mesylate | HCID 148757 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(Benzylthio)-2-nitroaniline | HCID 13550993 | — |
反応手順
To a solution of 19.5 g (0.1 mol) 4-thiocyano-2-nitroaniline in 130 ml dimethylformamide is added 3.78 g (0.1 mol) sodium borohydride, all at once. The mixture is stirred for one-half hour, then 15.2 g (0.1 mol) benzyl methanesulfonate in 70 ml dimethylformamide is added. The solution is stirred at 30° for 3 hours, cooled and partitioned between water and dichloromethane. The layers are separated and the aqueous phase reextracted with dichloromethane. The organic phases are combined, washed with aqueous K2CO3, water and saturated NaCl, dried, filtered and stripped to yield 4-(benzyl)sulfenyl-2-nitroaniline.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04145433 |
| 出典データセット | uspto-grants-1979_03 |
| ORD ID | ord-9ca894cf666d453283d8aac483b14ef1 |
| 出典メモ | uspto-grants-1979_03 |