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乙酐 → Acetic acid, ion(1-) (8CI,9CI)
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 乙酐 | HCID 7918 | — |
| 反应物 | 高氯酸 | HCID 24247 | — |
| 反应物 | 碳酸氢钠 | HCID 516892 | — |
| 反应物 | 13-methyl-17alpha-ethynyl-3-methoxygona-2,5(10)-dien-17-Ol | HCID 86733826 | — |
| 溶剂 | 乙酸乙酯 | HCID 8857 | — |
| 产物 | Acetic acid, ion(1-) (8CI,9CI) | HCID 175 | — |
| 产物 | 炔诺酮 | HCID 6230 | — |
反应步骤
Prepare a fresh solution of acetic anhydride (4.8 ml.) and 70% aqueous perchloric acid (0.01 ml.) in ethyl acetate (50 ml.) then add dl-13-methyl-17α-ethynyl-3-methoxygona-2,5(10)-dien- 17-Ol (0.5 g.) as a solid, swirl for 1.5 minutes then quench the reaction by adding saturated aqueous sodium bicarbonate solution. Wash the ethyl acetate layer with saturated bicarbonate, brine and dry over anhydrous sodium sulfate. Filter, evaporate in vacuo then add methanol with a trace of pyridine and let stand for 2 hours. Evaporate in vacuo, pump dry then treat the residue in ether with decolorizing charcoal. Filter, evaporate and crystallize the residue from methanol to obtain dl-13-methyl-17α-ethynyl-17-hydroxygon-4-en-3-one, acetate.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US03975412 |
| 来源数据集 | uspto-grants-1976_08 |
| ORD ID | ord-4f3638211e3c4776a14f79af607aac78 |
| 来源说明 | uspto-grants-1976_08 |