Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → Ethyl 2-acetamido-1-benzothiophene-3-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2,3-Dichloro-5,6-dicyano-1,4-benzoquinone | HCID 6775 | — |
| 반응물 | 2-Acetylamino-4,5,6,7-tetrahydrobenzothiophene-3-carboxylic acid ethyl ester | HCID 98682 | — |
| 용매 | Benzene | HCID 241 | — |
| 용매 | Sodium Bicarbonate | HCID 516892 | — |
| 생성물 | Ethyl 2-acetamido-1-benzothiophene-3-carboxylate | HCID 3722285 | 35.8% |
반응 단계
A solution of 1a (3.0 g, 11.24 mmol) in benzene (100 mL) was mixed with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (3.8 g, 16.85 mmol). The resultant mixture was heated at reflux for 2 h, diluted with saturated NaHCO3 solution (300 mL) and extracted with ethyl acetate (300 mL, 3×). The combined organic phases were dried over MgSO4, filtered, and concentrated. Flash chromatography (hexanes/ethyl acetate, 8:1) then provided the title compound (1.06 g, 35%) as a yellow solid: MS (ES) m/z 264 (M+H)+;
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07300952B2 |
| 출처 데이터셋 | uspto-grants-2007_11 |
| ORD ID | ord-ca82a885f0e3499ca73fc9c89411321a |
| 출처 메모 | uspto-grants-2007_11 |