Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethanethiol → 4-(2-carbethoxy-1-ethyl)-7-hydroxy-2-oxo-2H-1-Benzopyran
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethanethiol | HCID 6343 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 반응물 | 4-(2-carbethoxy-1-ethyl)-7-methoxy-2-oxo-2H-1-Benzopyran | HCID 86747239 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-(2-carbethoxy-1-ethyl)-7-hydroxy-2-oxo-2H-1-Benzopyran | HCID 12477114 | 27.1% |
반응 단계
To a suspension of 726 mg (5.4 mmol) of AlCl3 in 10 mL of dichloromethane at 0° C. was added 4 mL of EtSH. The suspension became a clear solution within seconds. Then, 298 mg (1.08 mmol) of 3 in 4 mL of dichloromethane was added, turning the yellow solution red in color. The ice bath was removed, and the reaction stirred to room temperature for 3 h. The solvents were removed in vacuo, and the residue thoroughly vacuum dried. The residue was extracted into EtOAc as much as possible, then the extract was flash chromatographed using 30/70 EtOAc/hexane. The long- and short-wave UV active band gave 76.7 mg (27%) of 4.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05247099 |
| 출처 데이터셋 | uspto-grants-1993_09 |
| ORD ID | ord-4f75d89850dd4de3a07f2755539ba444 |
| 출처 메모 | uspto-grants-1993_09 |