Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → Dibenzo(b,f)thiepin-1-carboxylic acid, 10,11-dihydro-8-methoxy-
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 2-Methoxy-9-cyano-10,11-dihydrodibenzo[b,f]thiepin | HCID 23337048 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | Dibenzo(b,f)thiepin-1-carboxylic acid, 10,11-dihydro-8-methoxy- | HCID 3045903 | 69% |
반응 단계
An amount of 6.0g potassium hydroxide was dissolved in 20ml of 80% ethanol and to the solution was added 1g of 2-methoxy-9-cyano-10,11-dihydrodibenzo[b,f]thiepin and the resulting mixture was refluxed for 26 hours. The mixture was freed of the solvent under reduced pressure to obtain the residue, which was dissolved in water and extracted with ethyl acetate. The aqueous layer was acidified with conc. hydrochloric acid and extracted with ethyl acetate. The extract was washed with saturated sodium chloride solution, dried over anhydrous sodium sulfate and freed of the solvent to give 743 mg (69%) of 2-methoxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin as pale reddish needles having a melting point of 185°-186° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04101667 |
| 출처 데이터셋 | uspto-grants-1978_07 |
| ORD ID | ord-78294fe96ff244f2a6ef9ec7869ed128 |
| 출처 메모 | uspto-grants-1978_07 |