Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → (3aR,6aR)-5-Methyloctahydropyrrolo[3,4-b]pyrrole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | tert-Butyl (3aR,6aR)-5-methylhexahydropyrrolo[3,4-b]pyrrole-1(2H)-carboxylate | HCID 44221715 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | (3aR,6aR)-5-Methyloctahydropyrrolo[3,4-b]pyrrole | HCID 44221716 | — |
반응 단계
To a solution of the product of Example 7A (20.8 g, 0.86 mole) in methanol (450 ml) was added aqueous 3N HCl (300 ml). The mixture was stirred at room temperature overnight, then concentrated to dryness at 30° C. under vacuum. The residue was treated with aqueous 1N NaOH to obtain a pH of 9-10. The mixture was concentrated to dryness. The crude material was purified by chromatography (eluting with a mixture of 10% methanol and 1% ammonium hydroxide in dichloromethane) to provide the title compound. 1H NMR (300 MHz, CDCl3) δ ppm 4.12-4.17 (m, 1H) 3.31-3.43 (m, 1H) 3.19-3.30 (m, 1H) 3.12 (d, J=11.53 Hz, 1H) 2.88-3.01 (m, 1H) 2.69 (dd, J=9.49, 2.37 Hz, 1H) 2.40-2.52 (m, 2H) 2.33 (s, 3H) 2.12-2.28 (m, 1H) 1.82-1.95 (m, 1H). MS: (M+H)+=127.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07728031B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-c832e9918ba14ed7beca1c88010d876d |
| 출처 메모 | uspto-grants-2010_06 |