関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | p-Bromobenzenesulfonyl chloride | HCID 7396 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-bromo-N-methylbenzene-1-sulfonamide | HCID 101215 | 96.8% |
反応手順
To a mixture of sat aq. NaHCO3 (42 g, 0.50 mol), CH2Cl2 (400 mL) and methylamine (51.7 g, 0.50 mol, 30% in methanol) was added a solution of 4-bromo-benzenesulfonyl chloride (130 g, 0.50 mol) in CH2Cl2 (100 mL). The reaction was stirred at 20° C. overnight. The organic phase was separated and dried over Na2SO4. Evaporation of the solvent under reduced pressure provided 4-bromo-N-methyl-benzenesulfonamide (121 g, crude), which was used in the next step without further purification. 1H NMR (CDCl3, 300 MHz) ε 7.65-7.74 (m, 4H), 4.40 (br, 1H), 2.67 (d, J=5.4 Hz, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08524767B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-3a3fa9322cb64c919ad2e855d9448eaf |
|---|
| 出典メモ | uspto-grants-2013_09 |
|---|
