참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | (+)-Estrone 3-methyl ether | HCID 92895 | — |
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 촉매 | Platinum | HCID 23939 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-Methoxyestra-1,3,5(10),9(11)-tetraen-17-one | HCID 12811166 | 83.9% |
반응 단계
A solution of 3.0 grams of 3-methoxy-13β-methylgona-1,3,5(10)-trien-17-one and 0.66 gram of sodium acetate in 60 milliliters of methanol and 20 milliliters of dichloromethane was electroyzed between the same platinum electrodes as specified in Example 1 while a potential of 1.7 volts (measured at the anode against a standard saturated calomel electrode) was maintained between the electrodes. At the completion of the electrolysis, which was established by thin-layer chromatography, the solution was made slightly acid by adding sulfuric acid thereto and it was allowed to stand at room temperature for a period between 20 and 30 minutes. Thereafter the dichloromethane was distilled and the product was crystallized from the remaining methanolic solution. In this manner, 2.5 grams of 3-methoxy-13β-methylgona-1,3,5(10),9(11)-tetraen- 17-one having a melting point of 142°- 145° C. was obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04029648 |
|---|
| 출처 데이터셋 | uspto-grants-1977_06 |
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| ORD ID | ord-db87d04916e1459f81bcb5a34c679656 |
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| 출처 메모 | uspto-grants-1977_06 |
|---|
