참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | 4-Nitro-2-sulfobenzoic acid | HCID 407025 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Methoxycarbonyl-5-nitrobenzenesulfonic acid | HCID 19693801 | — |
반응 단계
A suspension of 190.0 g (0.77 mol) of 2-carboxy-5-nitrobenzenesulfonic acid, 10 ml of DMF and 250 ml (3.43 mol) of thionyl chloride is heated at boiling for 3 h. After separating off the insoluble constituents by filtration, the filtrate is concentrated. 200 ml (4.94 mol) of methanol are added to the residue which results. When addition is complete the reaction mixture is cooled to 0° C. The solid which precipitates is filtered off and dried. 70.9 g (35.3% of theory) of colorless, crystalline 2-methoxycarbonyl-5-nitrobenzenesulfonic acid (m.p.: 92°-94° C.) are thus obtained. By distilling off the volatile components from the mother liquor, a second fraction (62.5 g, 31.1% of theory) is obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05723409 |
|---|
| 출처 데이터셋 | uspto-grants-1998_03 |
|---|
| ORD ID | ord-ef5dd0a2d9f54429bb4780c2b3d7888b |
|---|
| 출처 메모 | uspto-grants-1998_03 |
|---|