Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Carbonate → HCID 178513361, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 반응물 | 5-Cyanothiophene-2-sulfonamide | HCID 22019526 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 178513361 | HCID 178513361 | 58% |
반응 단계
A stirred mixture of 5-sulfamoyl-thiophene-2-carbonitrile [CAS-No. 519055-65-3] (0.31 g, 1.65 mmol), hydroxylamine hydrochloride (0.23 g, 3.31 mmol) and sodium carbonate (0.175 g, 1.65 mmol) in water (4.6 ml) and ethanol (1 ml) was heated under reflux conditions for 1.5 h. The reaction mixture was poured into water (50 ml) and extracted with ethyl acetate (3×100 ml). The combined organic layers were washed with brine (100 ml), dried (MgSO4) and evaporated. The crude product was purified by flash chromatography on silica gel (ethyl acetate/heptane) and crystallization (ethyl acetate/MeOH/hexane) to yield the title compound (0.21 g, 58%) as a white solid. MS (ISN) 220.1 [(M−H)−]; mp 189° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08093263B2 |
| 출처 데이터셋 | uspto-grants-2012_01 |
| ORD ID | ord-75fa1fe94c4a423d86b5ada7da837b82 |
| 출처 메모 | uspto-grants-2012_01 |