Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Anhydride → Acetate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | Perchloric Acid | HCID 24247 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 13-methyl-17alpha-ethynyl-3-methoxygona-2,5(10)-dien-17-Ol | HCID 86733826 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Acetate | HCID 175 | — |
| 생성물 | Norethindrone | HCID 6230 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US03975412 |
| 출처 데이터셋 | uspto-grants-1976_08 |
| ORD ID | ord-4f3638211e3c4776a14f79af607aac78 |
| 출처 메모 | uspto-grants-1976_08 |