참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Methyl(2-(morpholin-4-yl)ethyl)amine | HCID 14979282 | — |
| 반응물 | Methyl 3-(chlorocarbonyl)benzoate | HCID 15563901 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Methyl 3-(methyl(2-morpholinoethyl)carbamoyl)benzoate | HCID 66586820 | — |
반응 단계
Into a 100-mL round-bottom flask, was placed a solution of N-methyl-2-morpholinoethanamine (2.1 g, 13.12 mmol, 1.00 equiv, 90%) in dichloromethane (20 mL), and triethylamine (1.47 g, 14.55 mmol, 1.00 equiv). This was followed by the addition of a solution of methyl 3-(chlorocarbonyl)benzoate (3.3 g, 15.00 mmol, 1.20 equiv, 90%) in dichloromethane (10 mL) dropwise with stirring at 0-5° C. The resulting solution was stirred for 3 h at room temperature. The resulting solution was diluted with 100 mL of dichloromethane. The resulting mixture was washed with 1×30 mL of 10% sodium bicarbonate. The resulting mixture was washed with 1×30 mL of brine. The mixture was dried over sodium sulfate and concentrated under vacuum. The residue was applied onto a silica gel column with dichloromethane:methanol (20:1). This resulted in 4.4 g (99%) of methyl 3-(methyl(2-morpholinoethyl)carbamoyl)benzoate as a brown solid.
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-cfe97405300d4a2a85f5d5ccf8662c63 |
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| 출처 메모 | uspto-grants-2016_04 |
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