참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | 4-Chloro-2-nitroaniline | HCID 6979 | — |
| 반응물 | Benzenesulfonyl chloride | HCID 7369 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N-(4-Chloro-2-nitrophenyl)benzenesulfonamide | HCID 555628 | — |
반응 단계
To a solution of 2-nitro-4-chloroaniline (500 mg) and pyridine (2.1 ml in methylene chloride (10 ml), benzenesulfonylchloride (1.2 ml) was added dropwise at 0° C. under an atmosphere of argon. The reaction mixture was stirred for 3 days at room temperature. To the reaction mixture, water was added. The mixture was extracted with ethyl acetate. The organic layer was washed, dried over and concentrated under the reduced pressure. The reside was recrystallized from AcOEt-hexane mixture solvent to give the by-product. The mother liquor was concentrated under the reduced pressure. The residue was purified on silica gel column chromatography (AcOEt-hexane) and recrystallized from AcOEt-hexane mixture solvent to give the title compound (175 mg) having the following physical data.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06448290B1 |
|---|
| 출처 데이터셋 | uspto-grants-2002_09 |
|---|
| ORD ID | ord-233de6277ac44ef7b0f02fea12d39e9c |
|---|
| 출처 메모 | uspto-grants-2002_09 |
|---|