Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Tetrahydrofuran → (3beta,5beta,15alpha,16alpha)-15,16-Dihydro-3,5-dihydroxy-3'H-cycloprop(15,16)androsta-6,15-dien-17-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | 7alpha-Chloro-5,6beta-epoxy-3beta-hydroxy-15beta,16beta-methylene-5beta-androstan-17-one | HCID 13075966 | — |
| 촉매 | Zinc | HCID 23994 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | (3beta,5beta,15alpha,16alpha)-15,16-Dihydro-3,5-dihydroxy-3'H-cycloprop(15,16)androsta-6,15-dien-17-one | HCID 13075974 | 94.4% |
반응 단계
107.5 g of 7α-chloro-5,6β-epoxy-3β-hydroxy-15β,16β-methylene-5β-androstan-17-one is dissolved in 500 ml of acetic acid and 500 ml of tetrahydrofuran and, after the addition of 324 g of zinc dust in three portions, stirred at room temperature for 16 hours. The zinc is then filtered off, the filtrate is diluted with methylene chloride, and washed with sodium bicarbonate solution and water. After drying over sodium sulfate, the product is concentrated under vacuum. By trituration of the thus-obtained solid with ethyl acetate, 91.5 g of 3β,5-dihydroxy-15β,16β-methylene-5β-androst-6-en-17-one is produced, mp 196° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04614616 |
| 출처 데이터셋 | uspto-grants-1986_09 |
| ORD ID | ord-4f6f033bf183440a905cf0a17ebf7a0c |
| 출처 메모 | uspto-grants-1986_09 |