참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 4-Morpholinobenzylamine | HCID 2776458 | — |
| 반응물 | Tert-butyl 3-(3-(2-(4-(chlorocarbonyl)pyridin-2-yl)-4-(piperidin-1-yl)phenylcarbamoyl)benzylthio)propanoate | HCID 86705963 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 66586822 | HCID 66586822 | 133.3% |
반응 단계
Into a 50-mL round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed a solution of tert-butyl 3-(3-(2-(4-(chlorocarbonyl)pyridin-2-yl)-4-(piperidin-1-yl)phenylcarbamoyl)-benzylthio)-propanoate (120 mg, 0.20 mmol, 1.00 equiv) in tetrahydrofuran (10 mL), (4-morpholinophenyl)methanamine (68 mg, 0.35 mmol, 1.50 equiv), and DIPEA (32 mg, 0.25 mmol, 3.00 equiv). The resulting solution was stirred for 4 h at room temperature. An additional 68 mg of 4-morpholinophenyl)methanamine was added. The resulting solution was stirred for an additional 2 h at room temperature. The resulting solution was diluted with 10 mL of H2O. The resulting solution was extracted with 3×50 mL of dichloromethane and the organic layers combined. The resulting mixture was washed with 1×50 mL of brine, dried over anhydrous sodium sulfate, and concentrated under vacuum. This resulted in 200 mg of crude product as a yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09301951B2 |
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| 출처 데이터셋 | uspto-grants-2016_04 |
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| ORD ID | ord-1f5ad2b44c904578bb4066b6d556b4b1 |
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| 출처 메모 | uspto-grants-2016_04 |
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