Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloromethane → Ethyl (E)-4-[-2-(5,6,7,8-tetrahydro-5,5-dimethyl-8-(1,3-dithian-2-yl)naphthalen-2-yl)ethenyl]benzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | 1,3-Propanedithiol | HCID 8013 | — |
| 반응물 | Ethyl (E)-4-[2-(5,6,7,8-tetrahydro-5,5-dimethyl-8-oxo-2-naphthalenyl)ethenyl]-benzoate | HCID 12069038 | — |
| 용매 | Potassium Carbonate | HCID 11430 | — |
| 생성물 | Ethyl (E)-4-[-2-(5,6,7,8-tetrahydro-5,5-dimethyl-8-(1,3-dithian-2-yl)naphthalen-2-yl)ethenyl]benzoate | HCID 19695066 | — |
반응 단계
To a cold solution (0° C.) of 140 mg (0.40 mmol) of ethyl(E)-4-[2-(5,5-dimethyl-5,6,-dihydro-naphthalen-8(7H)-one-2-yl)ethenyl]-benzoate (Compound A2), in 6.0 mL of methylene chloride was added dropwise 130 mg (0.12 mL, 1.2 mmol) of 1,3-propanedithiol and 0.17 g (0.15 mL, 102 mmol) of borontrifluoride diethyl etherate. The reaction stirred between 0° C. and room temperature for 4 h. The mixture was diluted with aqueous sat. potassium carbonate, and extracted with ether (2×). The organic phase was washed with brine, dried over MgSO4 and then concentrated in vacuo. The crude product was purified by flash chromatography (silica, 10% ethyl acetate in hexane) to afford the title compound as a solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05723666 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-ccd6fb9e203040fbbcdbd667f32b7bf3 |
| 출처 메모 | uspto-grants-1998_03 |