Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → Ethyl (+/-)-2,3,4,5-tetrahydro-3a,9b-butano-1H-benz[g]indole-1-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Ethyl (+/-)-[2-(3',4'-dihydro-2'-hydroxyspiro-[cyclopentane-1,1'(2'H)-napthalen]-2'-yl)ethyl]-carbamate | HCID 86745264 | — |
| 생성물 | Ethyl (+/-)-2,3,4,5-tetrahydro-3a,9b-butano-1H-benz[g]indole-1-carboxylate | HCID 86745265 | 59% |
반응 단계
A solution of the product from Example 13 (1.68 g, 5.29 mmol) in 15 mL of 3:1 acetic acid/concentrated sulfuric acid (v/v) was stirred at room temperature for 18 hours. The reaction mixture was poured into water (50 mL) and the resulting mixture was extracted with CH2Cl2 (4×30 mL). The combined organic extracts were dried (MgSO4), filtered and concentrated. The residue was dissolved in CH2Cl2 (100 mL and washed with saturated aq. bicarbonate solution (30 mL). The organic phase was dried (MgSO4), filtered and concentrated. The residue was purified by chromatography (silica gel, 9:1 heptane/ethyl acetate) to give the title compound (0.94 g, 59%) as a white solid mp 67°-69° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05070093 |
| 출처 데이터셋 | uspto-grants-1991_12 |
| ORD ID | ord-cd260806412b4d5ebad6b73b7513bf0c |
| 출처 메모 | uspto-grants-1991_12 |