참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Lithium Hydroxide | HCID 3939 | — |
| 반응물 | Ethyl orthoformate | HCID 31214 | — |
| 반응물 | 2-amino-N-methyl-5-(5-methylhexahydropyrrolo[3,4-c]pyrrole-2(1H)-yl)benzamide | HCID 69928598 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | HCID 69928688 | HCID 69928688 | — |
반응 단계
2-Amino-N-methyl-5-(5-methylhexahydropyrrolo[3,4-c]pyrrole-2(1H)-yl)benzamide (Intermediate 8A) (100 mg, 0.36 mmol) was dissolved in triethoxymethane (1 mL) and sealed in a microwave vial. Heated at 160° C. for 10 minutes. Reaction allowed to cool to room temperature and lithium hydroxide solution added (0.5 mL, 1M in methanol) and reaction stirred overnight. Organic layer loaded onto a 1 g SCX cartridge. The crude material was purified by SCX, and the solvent removed under reduced pressure. The crude material was then re-dissolved in methanol (1 mL) and purified by preparative-HPLC. Purified sample was free-based using 500 mg SCX cartridge to afford 3-methyl-6-(5-methylhexahydropyrrolo[3,4-c]pyrrole-2(1H)-yl)quinazolin-4(3H)-one (56 mg, 0.2 mmol).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08841289B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-7d2bf6bfb9384f03b91ce19946d24598 |
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| 출처 메모 | uspto-grants-2014_09 |
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